*Corr. Author’s Address: Wroclaw University of Science and Technology, Faculty of Mechanical Engineering, Department of Metal Forming, Welding Technology and Metrology, Lukasiewicza 7-9, 50-371 Wroclaw, Poland, marzena.lachowicz@pwr.edu.pl 493 Strojniški vestnik - Journal of Mechanical Engineering 68(2022)7-8, 493-505 Received for review: 2022-03-31 © 2022 The Authors. CC BY 4.0 Int. Licensee: SV-JME Received revised form: 2022-05-30 DOI:10.5545/sv-jme.2022.142 Original Scientific Paper Accepted for publication: 2022-06-01 Effect of Dual-stage Ageing and RRA Treatment on the Three-body Abrasive Wear of the AW7075 Alloy Lachowicz, M.M. − Leśniewski, T. − Lachowicz, M.B. Marzena M. Lachowicz * − Tadeusz Leśniewski − Maciej B. Lachowicz Wroclaw University of Science and Technology, Faculty of Mechanical Engineering, Poland The paper presents an analysis of the influence of the heat treatment state on the abrasive wear of the AW7075 aluminium alloy. To determine the hardening state, the material hardness was measured. It was found that hardness is not the only factor that influences this type of wear. For this reason, the influence of the emerging microstructure is also analysed in the considerations. After tribological tests, microscopic observations of surface features were carried out to determine the dominant mechanisms of surface damage. The results were extended by the hardness distribution carried out on the cross-section. There were no changes in hardness that could be related to either strain hardening or structural changes caused by friction. Keywords: aluminium alloys, AW7075, abrasive wear, heat treatment, hardness, microstructure Highlights • The hardness of the AW7075 alloy is not the only determinant of abrasive wear; with the microstructure of the tested alloy and the related heat treatment, the state also plays an important role in this respect. • The abrasive wear of the tested alloy can be ranked in the following order according to the heat treatment condition: dual ageing < RRA treatment < T6 state. • The wear features show a similar type of damage, regardless of the heat treatment state. Scratches, grooves, microcracks, and slight plastic deformation features be observed on the wear surface. • Decohesion developed mainly around grain boundaries and interfacial boundaries, which facilitates the loss of continuity with the matrix in the presence of coherent particles. Larger and incoherent precipitates in the matrix can act as an abrasive and increase the wear rate. • The presence of large particles of the primary phases, which do not dissolve at the stage of heat treatment, promotes their crushing and defragmentation during abrasive wear. • The surface hardness does not change due to the occurrence of mechanical effects resulting from friction. 0 INTRODUCTION There is relative movement between surfaces of components in some applications of aluminium alloys. Wear resistance then becomes an important property to consider. Numerous research studies show that heat treatment can have a significant impact on tribological wear. In particular, the fragmentation of the microstructure components can significantly affect the obtained tribological parameters [1] to [3]. The presence of intermetallic phases in the microstructure offers a wide spectrum of possibilities for the strengthening of aluminium alloys. This group also includes the high-strength 7000 series alloys. Two treatments are used for this purpose: supersaturation and subsequent ageing. The sequence for ageing the 7000 series alloys is given as follows: solid solution (a) → Guinier-Preston (GP) zones → η’ (MgZn 2 ) → η (MgZn 2 ) [4] and [5]. The typical hardness- ageing diagram for a heat-treatable aluminium alloy is shown in Fig. 1. GP zones are formed during ageing at room temperature or the early stages of ageing. They are fully coherent with the matrix. The greatest hardening effect is achieved at the stage of separation of the intermediate phase, which is related to the change in the mechanism of the interaction of the precipitates with dislocations. This is a typical T6 state. The stresses that are needed to cut the particles by dislocation, as well as the stresses caused by the Orowan mechanism associated with the formation of a dislocation loop around these precipitates, obtain their maximum values. The material hardness drops significantly when there is a complete loss of the coherence of the precipitates. Ageing to the T6 state is associated with a continuous distribution of grain boundary precipitates (GBPs) [6] and [7]. A properly carried out heat treatment should end at the stage of forming the matrix of precipitates (MPs), which is partially coherent with the intermediate phase η'. The T6 state is characterized by high strength and hardness but is highly susceptible to stress corrosion cracking. When looking for greater resistance to this type of corrosion, dual-stage ageing (DA) and Retrogression and Re-Ageing (RRA) treatment are used [9] to [13]. The first stage of DA ageing is characterized by a lower temperature when compared Strojniški vestnik - Journal of Mechanical Engineering 68(2022)7-8, 493-505 494 Lac ho wicz, M.M. − Leśnie wski, T . − Lac ho wicz, M.B. to conventional ageing, and it is responsible for the diffusion and homogeneous distribution of the GP zones. The coarse-grained GP zones and phases are formed during the second ageing and contribute to the peak hardness. MPs are coarser and partially incoherent with phase η when compared to one- step ageing. This helps to reduce the hardness of the alloy [12] and [13]. Another solution is the multi- stage RRA heat treatment. Retrogression involves heating the alloy, which had earlier been hardened, at a temperature in the range of 200 ºC to 260 ºC for a short period (120 s), and then re-ageing the alloy to a condition typical for the T6 state. The use of the RRA treatment leads to the obtaining of a microstructure that is characterized by the presence of fine-dispersed and coherent η’ (MgZn 2 ) MPs. They are characteristic of the T6 state. However, at the GBPs there are fragmented and discontinuous precipitations that are typical for T7 over-ageing. As a result, the grain boundary that is line blocked with continuous GBPs particles, as in the T6 state, is transformed into a state in which the precipitates of the η phase are coarse and discontinuous [9], [14], and [15]. After the RRA treatment, a larger fraction of the GBPs was observed [7]. Also, the copper content of GBPs increases with the time of heat treatment [6]. Fig. 1. Schematic illustration of the precipitate strengthening contributions as a function aging time (based on [8]) The effect of heat treatment of aluminium alloys on their strength is already known. Its influence on the resistance to structural corrosion is also well understood [12] to [16]. Retrogression and re-ageing treatment improve the resistance to stress corrosion cracking (SCC) [6], while maintaining high strength, until the MPs become coarse [6]. However, the microstructure changes caused by heat treatment affect other functional properties of aluminium alloys. The high strength is maintained as long as the MPs are not coarse [6]. The RRA state is characterized by high resistance to fatigue crack initiation and better impact toughness as a result of the increased discretion of the precipitates occurring at the grain boundaries [9], [17] and [18]. Coarse GBPs also increase electrical conductivity [9]. The DA state, in terms of microstructure, brings the alloy closer to the over-ageing condition, which in turn results in a reduction in strength and an increase in ductility [19]. It seems obvious that the different hardnesses obtained for individual states should also affect the tribological wear. For this reason, in the present study, it was decided to consider the influence of microstructure on the abrasive wear of the AW 7075 aluminium alloy. 1 MATERIAL AND METHODS The tests were carried out on the AW 7075 aluminium alloy. The chemical composition of the alloy, which was determined by GDS-500A Leco glow discharge optical spectrometry (GD OES), is shown in Table 1. In the microstructure of all the tested samples, α(Al) solid solution was observed with grey, large precipitates of the α-AlFeMnSi phase, and dark primary precipitates of the Mg 2 Si phase (Fig. 2). The type of these particles was determined on the basis of the EDS results conducted as part of the preliminary studies and compared with the literature data. The grains of the solid solution were heterogeneous in nature and were surrounded by large precipitates of the iron-rich phase. The main changes in the microstructure, which were caused by the applied heat treatment, concern the morphology, size, quantity, and coherence of the formed precipitates. For this reason, the microstructure of the material in the image of the light microscope was of a similar nature. These changes are subtle and can, therefore, only be observed with the use of transmission electron microscopy (TEM) methods. However, it can be seen that in the case of the DA state, the precipitations of the strengthening phases are more clearly visible, which indicates their larger dimensions. Table 1. Chemical composition of the tested AW7075 aluminium alloy Element Zn Mg Cu Fe Cr Si Mn Ti Al Content [%] 5.42 2.34 1.45 0.39 0.26 0.12 0.10 0.03 rest Strojniški vestnik - Journal of Mechanical Engineering 68(2022)7-8, 493-505 495 Effect of Dual-stage Ageing and RRA Treatment on the Three-body Abrasive Wear of the AW7075 Alloy The parameters of three various heat treatments were developed for 30 mm × 100 mm sections with a thickness of 10 mm that were cut from the tested alloy (Fig. 3). The microstructure was investigated on conventionally prepared metallographic microsections using a Leica DM6000M light microscope. The tests were carried out before and after etching with a 10 % aqueous solution of HF. To determine the material hardening, BHN hardness measurements were carried out using the Brinell method and a DuraJet G5 hardness tester (Struers). To determine the abrasive wear resistance, tests were carried out on the T-07 tester made at the Institute of Sustainable Technology in Radom (Poland). The tribological tests were performed in the presence of the loose F90 electro-corundum abrasive, and all the tested samples were subjected to the same friction conditions. The used abrasive reflects the penetration of aluminium oxide or anodic coatings into the friction area very well. The oxide film is thin and can break off easily, in turn producing wear debris particles. The removal of the protective layer also accelerates the corrosive effects [20]. The method complied with the requirements of the GOST 23.208-79 standard [21]. The tested system consisted of a sample (plate) made of the tested material, and a counter-sample (roll) with a rubber ring. During the test, the material sample was pressed with a defined force of (F N ) to a rubber disk with a diameter of d = 50 mm, which was rotating at a constant speed (n). Gravity was used to deliver a loose abrasive between the rotating disc and the fixed sample. In the presence of loose abrasive, the sample of the tested materials and the reference sample were subjected to abrasive wear under the used operating conditions, i.e., rotational speed n = 60 rpm/min, test time t, and F N loads in accordance with the above standard (t = 10 min, F = 44 N). The reference sample was grade C45 normalized steel. Next, the mass loss of the reference sample (Z ww ) and the mass loss of the tested materials (Z wb ) were a) b) c) Fig. 2. Microstructure after; a) T6, b) DA, and c) RRA, light microscopy, etched with 10 % HF Fig. 3. Flow chart for the heat treatment process; a) T6, b) DA, and c) RRA Strojniški vestnik - Journal of Mechanical Engineering 68(2022)7-8, 493-505 496 Lac ho wicz, M.M. − Leśnie wski, T . − Lac ho wicz, M.B. determined. The mass loss of the samples (weight difference before and after the tests) was determined after a defined test time (determined by the number of rotations of the rubber roller). Based on the mass loss measurements, the abrasive wear resistance index K b (relative wear resistance) was calculated from the following equation (Eq. (1)): K ZN ZN b ww bb wb ww      , (1) where Z ww is the mass loss of the reference material (C45 steel), Z wb the mass loss of the tested material, ρ w the density of the reference material, ρ b the density of the tested material, N w the number of revolutions of the reference material’s friction path, and N b the number of revolutions of the tested material’s friction path. The density of the tested material (AW 7075) was 2.81 g/cm³. The morphology of the specimens after the tribological tests was observed using scanning electron microscopy (SEM), which also identified the wear features. The Phenom World ProX microscope was used for this purpose. Backscattered electrons (BSE) and second electrons (SE) detectors with an accelerating voltage of 15 kV were used. 2 RESULTS AND DISCUSSION 2.1 Hardness Measurements Based on the performed measurements, it can be stated that the proposed heat treatment contributed to the material strengthening (Fig. 4). It was found that the Brinell hardness (BHN) of the AW7075 alloy increases in the following order: DA