Structure and properties of aluminium–magnesium casting alloys after heat treatment
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Abstract
Since the forming of the microstructure depends on the specific of the casting method, which directly affects further mechanical and physical properties of the material, it is important to understand how to control the microstructure of the cast to understand changes that taking place during the crystallisation process. For estimating the metallurgical quality of the liquid metal before casting, the thermal-derivative analysis (TDA) is utilised. The TDA has been used for a long time, in both ferrous and non-ferrous industries casting. The Universal Metallurgical Simulator and Analyser (UMSA) platform is a rapid, sensitive and economical method of determining a full range of solidification features. The work focuses on the thermal analysis and heat treatment of aluminium alloys. The liquidus and solidus temperatures and dendrite coherency point (DCP) are then characterised. The research shows that the UMSA platform allows precise determination and calculation of thermal parameters. The influence of the heat treatment on structure and properties of aluminium castings has been determined as well. Heat treatment was carried out to increase the mechanical properties of aluminium alloys. Based on the findings above, the influence of microstructure on properties of the alloys is discussed.
Keywords
Thermal-derivative analysis Dendrite coherency point Heat treatment Structure Aluminium alloy Tensile propertiesIntroduction
Aluminium–magnesium casting alloys have a wide range of application, especially in the automotive and shipborne industry that is directly related to their good mechanical properties [1, 2]. These alloys are characterised by relatively good castability and are distinguished by excellent corrosion resistance due to high magnesium content [3, 4]. However, application of aluminium casting alloys for structural components requires high strength and suitable high elongations. Grain size, their morphology, interdendritic distance and distribution of secondary phases are crucial factors affecting mechanical properties of cast parts [1, 5, 6, 7]. The quality of the microstructure of aluminium alloys mainly depends on the chemical composition, melting process and cooling rate [7, 8, 9]. Due to those facts, it is important to understand how to control structure forming of aluminium alloys through casting or heat treatment.
The grain size of alloys related closely to their solidification characteristics under equilibrium and non-equilibrium conditions. Due to its comfort of use and inexpensive cost, thermal-derivative analysis (TDA) is much more suitable for industrial applications related to other thermal techniques and TDA method has been successfully used to analyse the features of aluminium, magnesium and zinc alloys in recent years [10, 11, 12]. In this method, the temperature changes in the sample are recorded from wholly liquid to completely solidified phases creating a curve plot of temperature as a function of time. A cooling curve reflects the release of latent heat of solidification. This release of latent heat in multicomponent alloys changes the slope of the cooling curve which is then used to detect the characteristics of transitions and phase reactions during solidification [11, 12, 13]. The solidification characteristics, e.g., dendrite nucleation and dendrite coherency, can be derived from thermal analysis of the alloy solidification. The dendrite coherency point temperature refers to the state of solidifying alloys at which a coherent dendrite network is established through the formation of grains. Once the dendrites become coherent, liquid metal flow is restricted to interdendritic regions. There exist four main DCP temperature testing approaches: the rheological technique (however, this method may influence DCP measurement), thermal analysis of the minimum temperature differences between two cooling curves, thermal analysis of the second derivative of cooling curve and the thermal diffusivity measurements techniques [12, 14].
The dendrite coherency point (DCP) temperature refers to the state of a solidifying alloy at which a coherent dendrite network is established during the formation of grains. In agreement with this understanding, the grain size in solidifying microstructure has been decided and will not change at/after this point. Correspondingly, the solid fraction (f) at DCP has been defined as f DCP, and a higher f DCP means finer grain size after solidification of alloy [14].
Specialists have been working for many years to improve mechanical properties of light alloys through the microstructure controlling using special casting techniques (sand casting, high-pressure die casting, mould casting), adding micro-additions that cause obtaining fine-grained microstructure, applying surface treatments or using heat treatment that should ensure increase in material properties [15, 16, 17].
The presented investigation was initiated to determine an influence of heat treatment on the structure and properties of EN AC 51100 and EN AC 51300 alloys. The first stage of the experiment was to examine the influence of cooling rate on the solidification process in studied alloys. The second stage was determination of the most beneficial type of heat treatment based on the mechanical examinations such as hardness measurements and static tensile test.
Experimental
Material
Chemical composition of investigated alloys/mass/%
| Mg | Si | Fe | Cu | Al | |
|---|---|---|---|---|---|
| EN AC 51100 | 2.86 | 0.07 | 0.07 | 0.01 | Bal |
| EN AC 51300 | 5.55 | 0.08 | 0.07 | 0.01 | Bal |
Metallographic investigations
The metallographic studies of EN AC 51100 and EN AC 51300 alloys were made on the as-cast samples taken from the ingot and on samples after solution treatment and artificial ageing. The change of the microstructure of samples subjected to different types of heat treatment has been investigated. Specimens were cold mounted and ground on 240#, 320#, 400#, 600# and 1200# SiC abrasive and then finished with 6-, 3- and 1-μm diamond paste. To reveal microstructure prepared specimens were etched using Keller’s reagent (0.5 mL HF, 1.5 mL HCl, 2.5 mL HNO3, 95.5 mL H2O) and Weck’s reagent (4 g KMnO4, 1 g NaOH, 100 mL H2O) immersed for 60 s. To obtain grain contrast, the polished samples were subjected to electrolytic etching using Barker’s reagent (5 mL HBF4 (40 %), 200 mL H2O) under a current of 20 V and then observed under bright field and polarised light (using sensitive tint). The microstructure of characteristic states of investigated alloy was observed using an optical microscope Axio Observer Image Analyser.
Thermal analysis
The thermal analysis through melting and solidification sequences was performed using the Universal Metallurgical Simulator and Analyser (UMSA) [13]. The melting and solidification trails for the aluminium alloy were performed using argon as cover gas. The data for thermal analysis (TA) was gathered using a high-speed National Instruments data acquisition system linked to a personal computer. The recorded data were imported into Fityk for data analysis. The cooling curves and corresponding derivative curves were plotted to determine characteristic thermal events, based on the first and second derivative of cooling curve. To ensure the reproducibility of testing results, a thermal analysis of each alloy was performed at least three times. The procedure consisted of following steps. First, the test specimen was heated to 700 ± 2 °C and isothermally held at this temperature for 90 s to stabilise the melt conditions. Next, the test sample was solidified at a cooling rate of approximately 0.5 and 0.9 °C s−1 that was equivalent to the solidification process under natural and accelerated cooling conditions.
For the determination of solid fraction at DCP, the Newtonian baseline has been estimated by sixth polynomial fitting (dT/dt)BL = a 0 + a 1 T + a 2 T 2 + a 3 T 3 + a 4 T 4 + a 5 T 5 + a 6 T 6 between the beginning and the end of solidification in the first derivative curve. The sixth-order polynomial yields a correlation coefficient >0.99. The solid fraction at DCP was calculated from the accumulative area between the first derivative and the baseline at t DCP as a fraction of the area between these curves.
Heat treatment
The solid solution temperature of EN AC 51100 and EN AC 51300 alloy was selected experimentally and based on the results obtained from the thermal-derivative analysis (UMSA). The test samples were heated for 8 and 12 h in the furnace in a wide range of temperatures and then immediately cooled in cold water. The influence of solid solution hardening and the artificial ageing mechanism of EN AC 51100 and EN AC 51300 alloys was precisely investigated. The temperature of artificial ageing was 160 °C. To analyse the influence of ageing time on the ageing potential of studied alloys hardness and tensile test measurements were taken.
Mechanical properties
To determine mechanical properties of the examined alloys, the test pieces were deformed in a static tensile test using universal tensile testing machine ZWICK Z/100 according to standard PN-EN 10002-1:2004. The hardness was measured using Automatic Rockwell hardness tester ZWICK ZHR 4150 under a load of 60 kg. Tensile tests and hardness measurements were carried out on the as-cast samples, after solution treatment and after various numbers of artificially aged specimens. To obtain precise results, ten hardness measurements were taken on each sample.
Results and discussion
Structure
Microstructure of a EN AC 51100, b EN AC 51300 alloy in as-cast condition observed in polarised light
Microstructure of EN AC 51100 in as-cast condition a etched using Keller’s reagent, b etched using Weck’s reagent (bright field)
Microstructure of AlMg3 alloy after precipitation treatment observed under a bright field (Keller’s reagent), b polarised light (Barker’s reagent)
Representative microstructure of the EN AC 51300 alloy after thermal analysis at cooling rate a 0.5 °C s−1, b 0.9 °C s−1
Results of grain size measurement of examined aluminium alloy after precipitation treatment
| Investigated alloys | Cooling rate/°C s−1 | Average grain size/µm |
|---|---|---|
| EN AC 51100 | 0.5 | 577 |
| 0.9 | 483 | |
| EN AC 51300 | 0.5 | 565 |
| 0.9 | 464 |
Thermal analysis
Before starting to analyse the solidification path of aluminium alloy must be noted that the number of phases in the as-cast state (non-equilibrium) can be larger than the number under equilibrium conditions, but the sequence of solidification reactions is, in general, in agreement with the corresponding phase diagrams.
The Mg2Si phase widely determines the properties of examined aluminium alloys, so their interpretation should be started from the Al–Mg–Si phase diagram that is relatively simple and has been treated in the literature in sufficient detail. In the aluminium corner of the Al–Mg–Si system, the following phases are in equilibrium with the aluminium solid solution: Al3Mg2 and Mg2Si. The Al3Mg2 (sometimes designated as Al8Mg5) has an FCC structure with lattice parameter a = 2.82–2.86 nm. The Mg2Si phase has a cubic structure with lattice parameter a = 0.635–0.640. In almost all commercial alloys belonging to the Al–Mg–Mg2Si system, aluminium is primarily solidified, and then one of the binary eutectics is formed. The binary and ternary eutectics, involving the Al3Mg2 phase, can solidify in commercial alloys, only under non-equilibrium conditions. As presented in work [19], the Al3Mg2 phase is formed by precipitation from the aluminium solid solution upon cooling in the solid state; however, under real, non-equilibrium conditions, this phase can form during solidification as a result of eutectic reactions. In as-cast Al–Si alloys, the Mg2Si phase develops only as a result of non-equilibrium ternary eutectic result at 555 °C, and its amount is small (<1 vol.%), which makes its classification difficult in an optical microscope. In spite of the comparatively weak mutual solubility of Mg and Si in solid Al, it enables a significant effect of precipitation due to the formation of metastable coherent and semi-coherent modifications (\(\beta^{{\prime \prime }} , \beta^{{\prime }}\)) of the Mg2Si phase during ageing. Recent results showed that the mutual solid solubility of magnesium and silicon in aluminium fully depends on temperature, which requires strict remark of a heat treatment regime. In Al–Mg alloys containing more than 3–4 % Mg, no secondary precipitates of Mg2Si phase are formed due to the low solubility of Si in Al. Almost all silicon is bound in eutectic Mg2Si particles [19, 20, 21].
Representative cooling, crystallisation and base curves with characteristic points of crystallisation process of a EN AC 51100, b EN AC 51300 aluminium alloys solidified at 0.5 °C s−1
Non-equilibrium thermal characteristics of the EN AC 51100 and EN AC 51300 alloy test specimens obtained during solidification process at 0.5 and 0.9 °C s−1 solidification rates
| Point | Reaction | EN AC 51100 0.5/°C s−1 | EN AC 51100 0.9/°C s−1 | EN AC 51300 0.5/°C s−1 | EN AC 51300 0.9/°C s−1 |
|---|---|---|---|---|---|
| 1 | T NUC αDEN | 641.3 | 639.8 | 629.1 | 633.2 |
| 2 | T MIN αDEN | 638.0 | 637.1 | 625.2 | 623.0 |
| 3 | T DCP αDEN | 638.5 | 637.7 | 625.9 | 623.8 |
| 4 | T G αDEN | 638.8 | 638.2 | 626.5 | 624.1 |
| 5 | \(T_{{{\text{E}}\left( {{\text{Al}} + {\text{Mg}}_{ 2} {\text{Si}}} \right)}}\) | 574.8 | 571.1 | 550.7 | 544.7 |
| 6 | \(T_{{{\text{E}}\left( {{\text{Al}} + {\text{Al}}_{3} {\text{Mg}}_{2} } \right)}}\) | 563.1 | 561.1 | 436.3 | 435.2 |
| 7 | T sol | 520.1 | 509.5 | 416.7 | 411.8 |
Solidification starts at approx. 629–641 °C with the formation of aluminium grains. The α-Al dendrite nucleation temperature (T NUC αDEN ) (point 1) represents the point when the stable primary dendrites begin to solidify from the melt. The variation demonstrated this fact in the slope of the cooling curves and determined by the first derivative inflexion point. The liquidus temperature means the beginning of the fraction solid that, at this point, is equal to zero. Clearly, the nucleation event for Al dendrite takes place at higher temperatures with the lower content of magnesium in the alloy, i.e., T NUC αDEN was 641.3 °C for EN AC 51100, which shifted down to 629.1 °C for EN AC 51300 alloy. As is evident, for EN AC 51300 the dendrite nucleation temperature increased by approx. 4 °C with increasing cooling rate. It could be also seen that increasing cooling rate for EN AC 51100 alloy does not provide significant changes in nucleation temperature. The increasing nucleation temperature allows new crystals to form ahead of solidification, which means there are more nuclei with less potential for growth, and thus effective grain refinement should be expected [14].
Representative cooling and second derivative curves and associated fraction solid curve of the EN AC 51100 alloy solidified at a 0.5 °C s−1, b 0.9 °C s−1 and the EN AC 51300 alloy solidified at c 0.5 °C s−1, d 0.9 °C s−1
The second derivative of the cooling curve was used to determine the dendrite coherency point (Fig. 6). The first minimum value of the second derivative of the cooling rate is defined as the DCP, which indicates the transition from liquid to a liquid–solid state. After passing this point, dendrites continued to grow and become thicker with further melt cooling.
Influence of cooling rate and magnesium content on temperature at dendrite coherency point and fraction solid of investigated magnesium alloys
| Cooling rate/°C s−1 | 0.5 | 0.9 | ||
|---|---|---|---|---|
| DCP/°C | Fraction solid/% | DCP/°C | FS/% | |
| EN AC 51100 | 638.47 | 2.8 | 637.71 | 4.1 |
| EN AC 51300 | 626.51 | 3.7 | 623.81 | 8.4 |
Mechanical properties
Results of hardness measurement of EN AC 51100 alloy in as-cast state and after heat treatment
| Temperature/°C | Solution treatment time/h | Hardness (as cast)/HRF | Hardness (solution treated)/HRF | Hardness (ageing 160 °C)/HRF | ||
|---|---|---|---|---|---|---|
| 4 h | 8 h | 12 h | ||||
| 580 | 8 | 47 | 44.6 | 64.5 | 64.8 | 66.8 |
| 12 | 46.0 | 58.1 | 65.3 | 64.8 | ||
| 560 | 8 | 44.5 | 48.1 | 58.4 | 53.4 | |
| 12 | 45.0 | 47.7 | 58.3 | 61.3 | ||
| 540 | 8 | 47.3 | 46.5 | 50.6 | 48.3 | |
| 12 | 46.2 | 46.3 | 55.4 | 55.1 | ||
Results of hardness measurement of EN AC 51300 alloy in as-cast state and after heat treatment
| Temperature/°C | Solution treatment time/h | Hardness (as cast)/HRF | Hardness (solution treated)/HRF | Hardness (ageing 160 °C)/HRF | ||
|---|---|---|---|---|---|---|
| 4 h | 8 h | 12 h | ||||
| 560 | 8 | 66 | 67.8 | 70.7 | 69.7 | 71.6 |
| 12 | 65.9 | 73.4 | 75.4 | 74.5 | ||
| 540 | 8 | 68.7 | 66.6 | 66.4 | 66.7 | |
| 12 | 67.7 | 68.0 | 71.0 | 71.2 | ||
| 520 | 8 | 66.4 | 70.0 | 67.6 | 69.3 | |
| 12 | 68.4 | 66.1 | 67.1 | 68.8 | ||
The analysis of data obtained from hardness measurement allows judging that EN AC 51100 alloy has highest ageing potential. As it could be observed after solutionising from temperature 580 °C, there is a significant increase in hardness even after 4 h of artificial ageing. Further quench ageing results in a subsequent small increase in hardness, and after 12 h of artificial ageing the material exhibits the highest hardness. Lower temperatures of solid solution treatment do not allow obtaining such a significant increase in hardness, but it can be seen that after quenching from temperature 560 °C and ageing through 12 h it is possible to get similar results as earlier. During precipitation treatment of EN AC 51300 alloy, an only small increase in hardness was observed. It could be caused by too short solution treatment time that did not allow the full solution of Mg in a matrix of the alloy and subsequent precipitation from solid solution when the alloy was artificially aged. As it is presented in Table 6, solution treatment from temperature 560 °C and subsequent ageing for 12 h at 160 °C cause the highest increase in hardness about 14 % in comparison with as-cast state. Quenching from lower temperature results in obtaining considerably lower hardness independent of ageing time that affords conclusion that those heat treatments are not economical because they do not permit to achieving a significant increase in material properties.
Tensile properties of EN AC 51100 alloy after precipitation treatment
| Condition | UTS/MPa | A/% | Condition | UTS/MPa | A/% |
|---|---|---|---|---|---|
| Solution treated 580 °C, 8 h | 198.4 | 35.8 | Solution treated, 580 °C 12 h | 196.5 | 30.8 |
| Aged 4 h, 160 °C | 223.8 | 29.8 | Aged 4 h, 160 °C | 214.0 | 28.6 |
| Aged 8 h, 160 °C | 232.2 | 25.1 | Aged 8 h, 160 °C | 225.2 | 27.6 |
| Aged 12 h, 160 °C | 236.32 | 25.7 | Aged 12 h, 160 °C | 233.4 | 27.0 |
The influence of the solution treatment and ageing time on tensile strength of a EN AC 51100, b EN AC 51300 alloys
Tensile properties of EN AC 51300 alloy after precipitation treatment
| Condition | UTS/MPa | A/% | Condition | UTS/MPa | A/% |
|---|---|---|---|---|---|
| Solution treated 560 °C, 8 h | 264.3 | 28.3 | Solution treated 560 °C, 12 h | 264.8 | 30.3 |
| Aged 4 h, 160 °C | 265.8 | 32.5 | Aged 4 h, 160 °C | 265.4 | 34.0 |
| Aged 8 h, 160 °C | 267.0 | 34.4 | Aged 8 h, 160 °C | 270.0 | 33.3 |
| Aged 12 h, 160 °C | 269.3 | 30.5 | Aged 12 h, 160 °C | 264.3 | 30.5 |
Conclusions
- 1.
Structure examinations of presented aluminium alloys confirm the presence of phases that influence on the hardness of the material. It was also observed that many of precipitated phases during precipitation treatment are considerably lower in comparison with as-cast state that certifies that a lot of Mg stays in solid solution and during artificial ageing precipitated uniformly in the core material.
- 2.
The higher cooling rate causes a decrease of solidus temperature in investigated alloys, resulting in an extension of the crystallisation range approx. 9 °C for both analysed alloys.
- 3.
A solid fraction at the dendrite coherency point determined from the second derivative of cooling curve increases with increasing Mg content and cooling rate.
- 4.
Despite micro-additions presence, it was not seen any changes in crystallisation curve that certify forming phases that contain Si or Cu which is caused by too little mass fraction of these additions in investigated alloys.
- 5.
As a result of conducted heat treatment process with different parameters of temperature and time and based on the hardness measurement best types of precipitation treatment were selected to carry out tensile tests. It has been proven that heat treatment has a significant effect on the hardness and tensile strength EN AC 51100 alloy, but results in a decrease in ductility of the material; however, precipitation treatment of EN AC 51300 alloy resulted in only a slight improvement in mechanical properties that could be caused by too short time of solution treatment.
- 6.
Based on the investigation results presented above, optimum heat treatment conditions were selected. For the EN AC 51100 aluminium alloy solution treatment temperature and time were 580 °C and 8 h with artificial ageing for 8 h at 160 °C; however, in the case of the EN AC 51300 solution treatment temperature and time were 560 °C and 12 h with ageing treatment for 8 h at 160 °C.
- 7.
The thermal analysis of the heating cycle permits the development of an optimum two- and/or multi-step solution treatment capable of improving the dissolution of the soluble phases and which results in achieving significantly higher mechanical characteristics in slowly solidified section of the automotive components.
Notes
Acknowledgements
This publication was financed by the Ministry of Science and Higher Education of Poland as the statutory financial grant of the Faculty of Mechanical Engineering SUT.
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