Materials Science and Engineering A 478 (2008) 7176

Work hardening characteristics in Al base alloys with 12.6 and 45 wt.% Zn

F. Abd El-Salam a , M.M. Mostafa a , L.A. Wahab b , M.T. Mostafa a , Sh.M. Abd El-Aziz a,
a b

Department of Physics, Faculty of Education, Ain Shams University, Cairo, Egypt National Centre for Radiation Research and Technology, Nasr-City, Cairo, Egypt

Received 9 April 2007; received in revised form 17 May 2007; accepted 18 May 2007

Abstract The stressstrain curves were obtained for AlZn alloys of 12.6 wt.% Zn (alloy I) and 45 wt.% Zn (alloy II) with elements of purity (99.99). The monotonic shift of these curves towards lower ow stress and higher ductility was interrupted at the transformation temperatures 483 K (alloy I) and both 543, 603 K (alloy II). By increasing deformation temperature, Youngs modulus, Y, yield and fracture stresses, y and f , respectively, fracture time, tf , the coefcient of parabolic work hardening, , decreased while fracture strain, f , and dislocation slip distance, L, increased. From the obtained X-rays diffraction patterns the lattice strain, , crystallite size, , and dislocation density, , were obtained at different deformation temperatures around transformation. 2007 Elsevier B.V. All rights reserved.
Keywords: Stressstrain; Transformation temperature; Flow stress; Ductility; Lattice strain; Crystallite size

1. Introduction Zinc is sufcially available, but it is well known for the problems related to wet ability and corrosion and in very lible to oxidation [1]. Al is one of the suitable candidates which improve the oxidation resistance of Zn [2]. In metals and alloys, the hardening induced by forming a structure in which dislocation mobility is reduced may be due to the intersection of dislocations, interaction of dislocations with impurity atoms, the formation of second phase particles and ordering [3]. Theoretical investigation of binary AlZn system suggests that it has the tendency for the self-coordination leading to segregation. Also, the study of concentration uctuations in the long wavelength demonstrates that a degree of likeatoms pairing exists in AlZn system [1]. The formation of precipitates greatly increases the strength of an alloy because FrankRead dislocation sources are supposed to cause hardening of polycrystals due to the subsequent formation of dislocation pile-ups at grain boundaries.

The solution of AlZn alloys by rapid quenching from the -phase eld produces a very ne structure with grains of very high dislocation density [4] (Fig. 1). The sequence and mechanism of structure transformation in supersaturated solid solutions, was found [5] to start with the formation of the spherical and the ellipsoidal GuinierPreston Zones (GPZ), which are rich in solute atoms, coherent with the matrix and differ from each other in the thermal stability. The transformation of GPZ, produces the rhombohedral transition phase (R-phase) which while losing some coherency yields the Zn rich fcc -phase and nally the Zn-rich stable precipitates. These thermally induced structure variations affect largely the hardening parameters of the alloy. So, the aim of the present work is to investigate the temperature and structure dependence of the tensile characteristics of AlZn system including (12.6 and 45) wt.% Zn. 2. Experimental procedure The AlZn alloys of 12.6 wt.% Zn (alloy I) and 45 wt.% Zn (alloy II) were prepared from highly pure Al and Zn (99.99%). The ingots were homogenized at 643 K for 24 h then drawn into wires of diameter 0.7 mm.

Corresponding author. Tel.: +20 123649582; fax: +20 25524403. E-mail address: Shereen moh@yahoo.com (Sh.M. Abd El-Aziz).

0921-5093/$ see front matter 2007 Elsevier B.V. All rights reserved. doi:10.1016/j.msea.2007.05.071

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Fig. 1. AlZn phase diagram.

The samples were 5 cm long. Both alloys were annealed at 643 K for 2 h then rapidly quenched to room temperature (300 K) to retain the fcc -solid solution formed at 643 K. Stressstrain tests were applied to the samples of both alloys in the temperature range 300523 K for samples of alloy I, and up to 643 K for alloy II till fracture. A conventional-type tensile testing machine described elsewhere [6] was employed. The applied stress was gradually increased (with 30 s internal between two successive loadings) and the elongation was recorded with an accuracy of 105 m, immediately after applying the stress. The yield stress, y , is considered to be the stress corresponding to the rst deviation from linearity in the starting part of the stressstrain curve. The maximum stress, the sample can indure before fracture was taken as the fracture stress, f , and the corresponding strain was considered as the fracture strain, f . Property variations due to composition or thermal treatment are caused by structural variations. X-rays diffraction can provide accurate information about the internal state of a material after deformation. Philips X-ray unit (PW 3710) with generator (PW 1830) was used to obtain the diffraction patterns for both alloys, with beam of wavelength = 0.15406 nm. Applying the equation: cos 1 2 sin = + (1)

Fig. 2. The stressstrain curves at different working temperatures for: (a) alloy I and (b) alloy II.

The monotonic shift of these curves towards lower ow stress and higher ductility when increasing the deformation temperature is interrupted at 483 K for alloy I, and at 543, 603 K, for alloy II, respectively. The softening of the deformed samples at high deformation temperatures is revealed from the behaviour of the temperature dependence of the following hardening parameters: 1. A decrease of the stress per unit strain, / (Yongs modulus Y), keeping the stress constant in the starting part of the stressstrain part of the stressstrain curves for both alloys, Fig. 3a. 2. The decrease of yield stress, y , with increasing deformation temperature, Fig. 3b. 3. A decrease of the fracture stress, f , which is the last maximum stress applied to the sample before fracture, Fig. 3c. The decrease in fracture stress points to a decrease in fracture time, tf . 4. A decrease of the coefcient of parabolic work hardening, , obtained as [7]: = 2 (2)

where is the peak angle of a plane, the diffracted X-ray breadth, the crystallite size from which the dislocation density is obtained as = 1/2 , and is the lattice strain. Half the slope of the linear relation between ( cos )/ and (sin /) refers to the lattice strain , and the inverse of the intercept on the ordinates gives the average crystallite size , from which dislocation density is obtained. 3. Experimental results The stressstrain curves obtained for alloys I and II taken at different deformation temperatures in the temperature range specied for every alloy, is given in Fig. 2a for alloy I, and in Fig. 2b for alloy II.

which is given in Fig. 3d. 5. An increase in fracture strain, f Fig. 3e.

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Fig. 3. The temperature dependence of (a) Y, (b) y , (c) f , (d) , (e) f , (f) L, (g) UR , and (h) UF for alloys I, II.

6. Increased dislocation slip distance, L, Fig. 3f given as: L= G2 b 2 (3)

4. Discussion The phase diagram of AlZn system [7] given in Fig. 1, shows that the thermally induced structural variations take place in the working temperature range used here. So, the temperature dependence of the observed variations in the measured parameters prove that they are structure sensitive parameters. The strength of binary alloy increases with increasing second phase content which decreases the mobility of dislocations. At certain temperature the thermally induced phases will be in general of the same features whether they stem from a formation or a dissolution process. Hence, the controlling factor will be the existing amount of the phase and the nature of the surrounding matrix [3].

The shear modulus G, and Burgers vector b. In Fig. 3, it is generally observed that the marked variations in the measured parameters take place in the transformation temperature ranges around 483 K for alloy I and around 543 and 603 K for alloy II. Fig. 4 shows the relation between ( cos )/ and sin / given as representative examples in Fig. 4a for Al planes in alloy I, and in Fig. 4c for Zn planes in Alloy II. The obtained data of Fig. 4 are given in Table 1.

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Fig. 4. The relation between sin / and cos / for Al planes: (a) for alloy I, (b) for alloy II and (c) Zn planes for alloy II.

In view of the phase diagram, Fig. 1, heating both alloys at 643 K then quenching to room temperature in cold water yield specimens of solid solution composition for the two alloys with very ne structure, very high dislocation density and quite complex grain boundary structure [8]. This consists with the high fracture stress and less ductility observed at low temperature, Fig. 2. The ow stress decreases and the ductility increases at high deformation temperatures. In the solid solution which maintains excess quenched in vacancies in a supersaturated state there may exist some of the following interactions that may contribute to hardening such as: short and long-ranges, chemical, elastic or electrostatic and Snoek ordering. Heating the quenched alloy at temperature below the line of solubility gives rise to controlled precipitation of the sec-

ond phase with a high level of ductility and ne structure [4]. In the present work and according to the phase diagram of Fig. 1, alloy I is characterized by single structure transformation from the double phase ( + ) into the single solid solution phase which is indicated by the irregular behaviour at 483 K, Fig. 2a and the drop in Fig. 3ac, at this temperature. In alloy II, two anomalies in Fig. 2b and drops in Fig. 3ad and g take place at 543 and 603 K, respectively indicating the formation of the ( + ) double phase then the single -phase, which is in fair agreement with Fig. 1. The subsequent formation of -phase precipitates at higher temperatures due to the formation of GPZ besides the presence of dislocations causing climb or dislocation loops of vacancy type [9] formed from the retained quenched-in defects and the high induced dislocation density [4] might be the cause of the rst abnormal changes at 483 and 543 K for both alloys, respectively. The height of the peaks depends on the transformation temperature and Zn content in both alloys. The quenched samples of alloy II on heating at 603 K some internal processes are supposed to take place during heating such as the dissolution of GPZ, formation and transformation of R-phase into -phase and -phase which ends with the Znrich stable precipitates that become highly dispersed forming the solid solution -phase at 603 K. The strengthening effects taking place during isothermal deformation of quenched AlZn alloy may be due to the nucleation and growth of the precipitating phases from solid solution. This also comprises the dissolution of the solid solution in a deformed matrix by preferential precipitation on grain boundaries [10]. At temperatures above the transformation temperature, the behaviour of the measured parameters shows a softening behaviour which may be due to the dislocation activity [11] induced due to the thermal growth of precipitates which facilitate dislocation motion between the large and less number of precipitates. The mechanisms proposed for softening in the temperature range of the solid solution [12] are diffusion-controlled phenomena, such as dislocation climb and glide processes. Raising the deformation temperature enhances the dissolution of the incoherent -phase in the -phase matrix. The increased recovery of the vacancy-type defects enhances the rate of diffusion of solute atoms. Accordingly, the aging rate is increased and larger widely spaced precipitate particles are formed at higher temperatures. Hence for a given alloy composition the large particles will be less effective in holding up dislocations or inhibiting slip. This leads to

Table 1 Temperature dependence of lattice strain, average crystallite size, and dislocation density, , for both alloys Al planes (alloy I) Temperature (K) 443 483 523 0.00155 0.0011 0.0035 (A) 434.8 588.23 1250 (1010 /cm2 ) Al planes (alloy II) Temperature (K) 543 583 603 623 0.00055 0.00245 0.00135 0.00415 (A) 769.23 303.03 476.2 178.6 (1010 /cm2 ) Zn planes (alloy II) 0.0032 0.0021 0.0023 0.0014 (A) 227.3 333.3 312.5 476.2 (1010 /cm2 ) 19.3 9 10.2 4.4

5.29 2.9 0.6

1.7 10.9 4.4 31.3

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a strength fall and a ductile state with reduced ow stress, Fig. 2. At 543 K, the precipitated mixed ( + ) phase transformed into the mixed ( + ) phase is with Zn-rich -phase. At 603 K, the mixed ( + ) phase transforms into the fcc -solid solution. The irregularity in the sequence of the stressstrain curves at 543 and 603 K Fig. 2, and the marked variations in the measured parameters, Fig. 3, at these temperatures might be due to the coarsening of and grains associated with the dissolution of Zn and Al which takes place to satisfy the actual equilibrium composition [13]. Atomic rearrangements and internal stress resulting from the new Frank-Read sources formed due to a change of the specic volume of the sample which takes place during the rearrangements in the dislocation network at the dissolution and transformation temperature, Fig. 2. The deformation of Al and Al alloys by tension enhances jog formation and facilitates cross slip which is dominated in Al and Al alloys due to their high stacking fault energy [3]. Jogs of opposite clusters will be annihilated leading to a decrease in jog density. Accordingly dislocations mobility increases. This explains the observed decrease of the hardening parameters of Fig. 3 and increase of f and L with increasing deformation temperature due to both the dissolution of the incoherent -phase in the -matrix and the homogeneity of the distribution of Zn atoms in the -phase. This is associated with the dissolution of interphase boundaries which facilitates the motion of dislocations within the grains and make possible grain boundary sliding. At higher temperatures the observed softening consists with the decrease of the hardening parameters Fig. 3 and the corresponding increase in resilience and toughness given in Fig. 3. At 443 K, the lattice strain = 0.00155, dislocation density = 2.3 102 /m2 , in Table 1 are the higher values than those for 483 K or after transformation, 523 K, but shows the minimum crystallite size, 434.8 A, Table 1. It is clear that when and increase, the crystallite size decreases. Increasing temperature some obstacles annihilate reducing lattice strain and dislocation density which increases crystallite size . This is at the transformation temperature 483 K where = 0.0011, = 1.7 102 /m2 , and therefore, = 588.23 A, Table 1. Above transformation, 523 K where the matrix became homogeneous with the least strain, = 0.00035, and = 0.8 102 /m2 , enhanced process due to a degree of like-atoms pairing may exist in AlZn system [1] leading to high growth for crystallite size, 1250 A, Table 1. In alloy II, the formation of -phase increases the distortion in Al crystals, = 0.00245, = 0.03 102 /m2 , which decreases its crystallite size, = 303.03 A, Table 1. The difference in crystal types of Al (fcc) and Zn (hexagonal) may explain the inverse variation of crystallite size in Al and Zn crystals which reached their larger crystallite size Zn = 476.2 A. The temperature dependence of the lattice parameter, a, the half line width ( 2) of the -phase and the ratio, c/a, for phase are given in Fig. 5ac. Besides the strain hardening the hardening caused by Zn atoms represented by their large effect on the distribution of vacancy clusters and the existing precipitate, increase the hard-

Fig. 5. Temperature dependence of the average lattice parameter, a, the half line width, 2, for the -phase and c/a for -phase.

ness of the alloy and consequently increase the lattice parameter [14]. At 603 K, the peak value of the lattice parameter. A Fig. 5a, points to a high deformation level in the alloy with the result of high residual strain corresponds to the peak in, 2, Fig. 5b. This consists with the minimum crystallite size indicated through, c/a, Fig. 5c, for the -phase (Zn). At 613 K, the drop in Figs. 5a, b and 3ad and the increase in Fig. 3eh which corresponds to decreased lattice parameter indicates the occurrence of a recovery process due to the relief of the internal strains or stresses during the thermally activated growth of the stable incoherent -phase with larger crystallites. Above 613 K, the dissolution of the -phase associated with a high concentration of vacancies increases the lattice constant, a, Fig. 5a. Therefore the formation of -phase may lead to heterogeneities in the dissolution of -atoms in -phase showing a solid solution hardening.

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This increases the internal strain, 2, Fig. 5b, and decreases the ratio, c/a, Fig. 5c. 5. Conclusion 1. Al12.6 wt.% Zn alloy is characterized by single structure transformation at 483 K, while Al45 wt.% Zn alloy showed two transformations at 543 and 603 K. 2. The strengthening effect taking place during isothermal deformation of quenched AlZn alloy may be due to the nucleation and growth of the precipitating phases from solid solution. This comprises the dissolution of the solid solution in a deformed matrix by preferential precipitation on grain boundaries. 3. The softening behaviour of the measured parameters above the transformation temperature may be due to the dislocation activity induced due to the thermal growth of precipitates which facilitate dislocation motion between the larger and less number of precipitates. 4. The mechanisms proposed for softening in the temperature range of solid solution are diffusion-controlled phenomena such as dislocation climb and glide process.

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