Materials Characterization 46 (2001) 251 257

Structural parameters of 7020 alloy after heat treatment simulating the welding process
Marzena Lech-Gregaa,*, Sonia Hawryl Ckiewiczb,1, Maria Richertb,1, skia,2 Wojciech Szyman
a

Physical Metallurgy Laboratory, Light Metals Division, The Institute of Non-Ferrous Metals, ul Pil C sudskiego 19, PL-32-050 Skawina, Poland b University of Mining and Metallurgy in Krakow, al. Mickiewicza 30, 30-059 Cracow, Poland Received 28 December 2000; received in revised form 5 February 2001; accepted 13 February 2001

Abstract The study presents quantitative analysis of particle and grain size distributions in Al Zn Mg (7020) alloy subjected to a heat treatment simulating the welding process. Microstructural analysis was done by the APHELION program. Some significant quantitative changes in the size and distribution of particles as a function of the heat treatment temperature were observed. The changes were related to the process of growth, dissolution, and precipitation of new, fine particles from the solid solution. The heat treatment was observed to have no effect on the grain size and on the size of the largest particles visible under an optical microscope. These phenomena, which influence the strength hardening and residual stress fields decide the properties of the welded joints. D 2001 Elsevier Science Inc. All rights reserved.
Keywords: Al Zn Mg; Welding; Heat treatment; Quantitative analysis

1. Introduction For some years, a dynamic development of fast maritime transport has been observed. In many countries fast ships have taken over a considerable percent share of the transport of passengers, cars, and containers [1]. Aluminium alloys, the Al5Zn1Mg alloy included, are considered to be the material most suitable for construction of the fast ships. In Al
* Corresponding author. Tel.: +48-12-276-4088; fax: +48-12-276-4776. E-mail addresses: zwlech@cyf-kr.edu.pl (M. LechGrega), sonia@agh.edu.pl (S. Hawryl Ckiewicz), mrichert@agh.edu.pl (M. Richert). 1 Tel.: +48-12-617-3356; fax: +48-12-632-5615. 2 Tel.: +48-12-276-4088; fax: +48-12-276-4776.

Zn Mg alloys, the variable dissolution characteristics of zinc and magnesium in aluminium is of great practical importance as it enables the use of heat treatment, like solutioning and ageing; bringing an increase of the mechanical properties in final products (precipitation hardening) and, by contrast, there are some operations (e.g., welding) that may considerably reduce the mechanical properties of the material [2,3]. These alloys are characterized by a unique combination of features important for the shipbuilding industry, like high strength per mass unit, high corrosion resistance in potable water and in seawater, good machinability, weldability, and workability. Welding deteriorates the alloy behaviour in the heat-affected zone due to strong local overheating. This, in turn, causes changes in the size and distribution of precipitates [4].

1044-5803/01/$ see front matter D 2001 Elsevier Science Inc. All rights reserved. PII: S 1 0 4 4 - 5 8 0 3 ( 0 1 ) 0 0 1 3 3 - 4

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Table 1 Chemical composition (wt.%) of the material used in investigation Zn Mg Cu Si Fe Mn Ti Al 4.7% 1.2% 0.065% 0.230% 0.250% 0.300% 0.036% rest

A quantitative estimation of microstructural parameters and particle size has become possible owing to the development of modern research techniques that allow not only particle observations at extremely high magnifications but also statistical processing of the results obtained [5]. New possibilities have been created in quantitative analysis and evaluation of the size and distribution of particles in Al Zn Mg alloys, enabling more complete interpretation of changes in alloy microstructure and of the MgZn2 precipitation processes [6]. The aim of the study was to analyze the changes in particle size and mechanical properties that take place in Al Mg Zn alloys under the effect of varying conditions of a heat treatment simulating the welding process.

Fig. 1. Mechanical properties (tensile strength, yield strength, elongation, hardness) after annealing and 1-year natural ageing (II).

2. Experimental conditions The material used in this study was 7020 semicommercial aluminium alloy. The chemical composition of the material is given in Table 1. The typical heat treatment of 7020 aluminium alloy consists in quenching to 450C followed by a two-step artificial ageing at 90C/8 h + 145C/15 h. In our experiment, after such a treatment, the samples were annealed at 250C, 350C, and 450C, and then artificially aged at 100C for 10 min. The samples were next subjected to natural ageing for 1 year at room temperature. Also samples without previous annealing, subjected only to natural 1-year ageing, have been investigated. Such preparation of samples allows us to observe the evolution of structure and the precipitation process after a long time that simulates the real conditions in aluminium-welded sheet.
Table 2 Mechanical properties After annealing I Tensile strength (MPa) Ageing 250C 350C 450C 361 310 308 290 Yield strength (MPa) 304 156 158 142 Elongation (%) 10 19 18 Hardness (HB) 94 72 72 69 Stress, s (MPa) + 10.8 27.5 29.5 33.3

The strength, yield stress, hardness, residual stresses, and microstructure were investigated. The mechanical properties were tested on an Instron Machine, and the residual stresses were investigated on Strainflex PSF-2M equipment using an X-ray sin2y method. The microstructure was examined by means of optical microscopy (Neophot 2); transmission electron microscopy (TEM) was carried out using a Tesla BS 500 microscope and a JEM2010 ARP microscope [chemical analysis of particles was made by energydispersive spectrometry (EDS) technique]. Image analysis has been performed by computer on binary images using the APHELION program.

3. Results Table 2 shows the results of mechanical property measurements just after normal heat treatment, typical for 7020 aluminium alloy, and then after additional annealing and natural ageing over 1 year. Similar levels of mechanical properties after previous annealing at 350C and 450C has been found in both cases, i.e., after the heat treatment (I) and 1year ageing (II). In contrast to this, the level of hardening of the samples after 1-year ageing is considerably higher.

After annealing and 1-year natural ageing II Tensile strength (MPa) 381 412 399 398 Yield strength (MPa) 310 242 231 230 Elongation (%) 11 22 24 22 Hardness (HB) 111 102 100 100 Stress, s (MPa) 15.7 4 39.2

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Fig. 2. Histograms of particle size distribution in 7020 alloy observed under an electron microscope.

In both cases the level of hardening of the samples after previous annealing at 250C is higher the in

comparison samples annealed at 350C and 450C (Fig. 1).

Table 3 Parameters of particles observed under electron microscope in (0 6) 10 3 mm2 and (6 50) 10 3 mm2 class ranges Class range Percent Average particle Average particle Class range Percent Average particle Average particle fraction size in classes size 10 3 10 3 fraction size in classes size 10 3 10 3 (mm2) (%) 10 3 (mm2) (mm2) (mm2) (%) 10 3 (mm2) (mm2) Ageing 0 1.5 1.5 3 3 4.5 4.5 6 0 1.5 1.5 3 3 4.5 4.5 6 0 1.5 1.5 3 3 4.5 4.5 6 0 1.5 1.5 3 3 4.5 4.5 6 98.9 0.4 0.1 0.1 53.1 15.6 6.3 5.0 35.5 18.0 8.6 5.6 76.3 6.2 2.7 1.6 0.07 2.10 3.57 5.15 0.59 2.27 3.63 5.07 0.77 2.12 3.70 5.16 0.52 2.14 3.64 5.21 0.09 6 20.6 20.6 35.3 35.3 50 6 20.6 20.6 35.3 35.3 50 6 20.6 20.6 35.3 35.3 50 6 20.6 20.6 35.3 35.3 50 0.36 0.11 0.02 16 2.3 0.6 23.6 6.1 0.5 8.5 3.0 0.9 11.7 26.3 42.2 10.7 25.6 41.4 11.4 26.1 45.5 12.4 27.1 43.2 16.6

250C

1.44

13.6

350C

1.87

14.9

450C

0.82

18.2

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Fig. 3. Microstructure after (A) artificial ageing, (B) 250C annealing, (C) 350C annealing, and (D) 450C annealing.

Tensile residual stresses have been found in samples that were only aged. In all other cases compressive residual stresses appeared. In samples just after annealing (I) the highest residual stresses exist in samples annealed at 250C and 350C, by contrast to samples after 1-year natural ageing (II) in which the highest compressive residual stresses appeared in samples annealed 450C [1]. The size of particles observed in Al Zn Mg alloy by TEM (Fig. 2) depends very definitely on the temperature of annealing, simulating the conditions of welding. The results of statistical measurements of particle size carried out at three different temperatures of annealing (250 C, 350 C, and 450C) and after ageing are given in Table 3. After ageing, most numerous were the finest particles of a size of up to 1.5 10 3 mm2; their content was about 99%. The quantitative fraction of other precipitates after ageing was minimal (Table 3) and invisible in the diagram (Fig. 2). In the sample annealed up to 250C, corresponding to the largest distance from the weld, the content of the finest particles decreased to about 50%, at the expense of the increasing content of larger particles of

a size of (6 10) 10 3 mm2 (Table 3, Fig. 2). The average particle size in the sample annealed up to 250C was 1.44 10 3 mm2. After annealing at 350C, the quantitative fraction of the finest particles decreased even more,
Table 4 Parameters of particles observed under optical microscope Class range (mm2) Ageing 0 17 17 34 34 51 0 17 17 34 34 51 0 17 17 34 34 51 0 17 17 34 34 51 Percent fraction (%) 74.9 20.8 4.3 74.9 20.6 4.5 73.4 21.3 5.3 75.0 20.1 4.9 Average particle size in classes (mm2) 7.05 23.16 40.06 7.55 23.89 41.71 7.25 23.15 40.92 6.67 23.88 41.25 Average particle size (mm2) 11.45

250C

12.29

350C

12.21

450C

11.54

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Fig. 4. Histograms of particle size distributions in 7020 alloy observed under an optical microscope.

i.e., to 35%, with respect to the aged sample, while the content of larger particles increased to 23% (Fig. 2). The average size of the precipitates was 1.87 10 3 mm2. An interesting change occurred in the sample annealed at 450C. A considerable increase in the content of the finest particles up to about 76% was observed, combined with a significant decrease in the content of larger particles (Table 3, Fig. 2). The average size of the precipitates was 0.82 10 3 mm2 and, compared to the average size of the particles observed after annealing at 250C and 350C, was the smallest. The examinations by electron microscopy and by EDS proved that the finest particles with a diameter

of 0.07 10 3 mm (Table 3) were those of MgZn2 (Fig. 3B). It was stated, moreover, that the nucleation sites of MgZn2 particles were mainly elements like Zr, Cr, and Mn, the presence of which was revealed during examinations of the chemical composition (Fig. 3). In medium-size precipitates, i.e., in the range of (14 18) 10 3 mm2, on the other hand, the presence of elements such as Ti, Mn, Fe, Zr, and Si (Fig. 3C and D) was confirmed. Large precipitates visible under an optical microscope did not change their dimensions with varying parameters of the heat treatment; no significant change in the distribution of these particles was observed either (Table 4, Fig. 4). On an average, the size of large particle observed under an optical

Table 5 Parameters of grain sizes in (0 15) 103 mm2 and (15 100) 103 mm2 class ranges Class range 103 (mm2) 250C 05 5 10 10 15 05 5 10 10 15 05 5 10 10 15 Percent fraction (%) 63.5 17.7 8.8 65.0 15.8 7.0 61.7 17.1 8.2 Average grain size in classes 103 (mm2) 1.78 7.12 12.0 1.84 7.10 12.3 1.64 7.15 12.0 Average grain size 103 (mm2) 3.84 Class range 103 (mm2) 15 57.5 57.5 100 15 57.5 57.5 100 15 57.5 57.5 100 Percent fraction (%) 10 0 11.8 0.4 11.8 1.2 Average grain size in classes 103 (mm2) 24.5 25.7 59.7 27.0 79.8 Average grain size 103 (mm2) 24.5

350C

3.62

26.9

450C

3.71

31.7

Average grain size 103 (mm2) Ageing 7.68 250C 5.95 350C 6.39 450C 7.25

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Fig. 5. Histograms of grain size distributions in 7020 alloy observed under an optical microscope.

microscope was about 12 mm2 and then remained rather stable, which suggested that particles of this type were primary, nonsoluble precipitates based on ferrous manganese compounds (Fig. 4). This was further confirmed by microstructural examinations, which revealed that large particles were precipitates containing Fe, Mn, and Cr (Fig. 4). Irrespective of the applied heat treatment parameters, the size of the grains observed under an optical microscope did not change in any more significant way and amounted, on an average, to (3.6 3.8) 103 mm2 (Table 5, Fig. 5) [6].

fraction of particles from individual group sizes in the alloy. In particular, an analysis of the content of the smallest particles in the alloy microstructure enabled us to follow the MgZn2 compound precipitation process, identified from examinations of the chemical composition by the EDS technique. The data on the distribution of the volume content of MgZn2 compound in the alloy are very important because MgZn2 particles are responsible for the precipitation hardening of Al Zn Mg alloy and affect in a significant way its mechanical properties [2,3]. From the results obtained it can be seen that in the heat-affected zone the following processes take place: 1. coagulation of fine precipitates after solutioning from 250C, 2. dissolution of fine precipitates at 350C and coagulation of large particles after solutioning, 3. precipitation from solid solution of finely dispersed precipitates of MgZn2 after solutioning from 450C The run of the precipitation process is complex and depends not only on the heat treatment temperature simulating the welding process but also on the time of holding at room temperature, applied in the

4. Discussion of results The quantitative studies of particle size observed by TEM and by optical microscopy were carried out by the APHELION program. The use of this program enables quantitative computation of large sets and statistical data processing. The data obtained compiled in Tables 3 5 and in Figs. 2 5, confirm that, depending on the heat treatment parameters simulating the welding process of Al Zn Mg alloy, considerable changes occur in the distribution of precipitates and in the quantitative

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process of natural ageing. The dissolution and coagulation processes are also responsible for changes in hardening and residual stresses. The precipitation of particles proceeded most intensely on cooling from the annealing temperature. A large number of particles, in most cases placed on the grain boundaries, was supposed to be the factor hindering the growth of the grains that, in spite of high annealing temperatures, did not change their dimensions.

Acknowledgments This research was supported by Polish State Committee for Scientific Research (KBN) under Grant No. 7T08C00514. The authors also wish to thank Dr. A. Klyszewski for photo on TEM.

References
[1] Lech-Grega M, Richert M, Kl Cyszewski A. Structural evolution in the ageing of AlZnMg alloy after control heat treatment. Proceedings of the 10th Conference on Electron Microscopy of Solids, Warsaw, Poland, September 1999. pp. 243 6. [2] Ma T, den Ouden G. Heat-affected zone softening during arc welding of Al Zn Mg alloys. Int J Joining Mater 1996;8(10):105 10. [3] Mondolfo LF. Aluminium alloys: structure and properties. Met Mater 1971;5(10):95 124. [4] Bertini L, Fontanari V, Straffelini G. Influence of post weld treatments on the fatigue behaviour of Al-alloy welded joints. Int J Fatigue 1998;20(10):749 55. w: WNT, 1995. [5] Rys J. Stereologia materialow. Krako [6] Hawryl Ckiewicz S, Lech-Grega M, Richert M, Szyman ski W. Quantitative changes in structure parameters of 7020 alloy after heat treatment simulating the welding process. Proceedings of the 6th International Conference on Stereology and Image Analysis in Materials Science, Krakow, Poland, September 2000. pp. 167 72.

5. Conclusions 1. The results obtained have proved that the distribution and quantitative fraction of the precipitated particles of MgZn2 in the heat-affected zone of Al Zn Mg alloy change in pace with variations in the annealing temperature, related to a distance of the individual regions from the weld axis. 2. The largest amount of the finest particles of MgZn2 was observed in the zone annealed at 450C and closest to the weld axis. An increased number of MgZn2 particles in that zone occurred due to the secondary precipitation after solutioning from 450C. 3. Besides the small particles of MgZn2, in all the samples examined, medium-size particles formed by coagulation and large primary particles stable in size were observed to be present.