Benjamin Milkereit

Dissolution and Precipitation Behaviour during Continuous Heating of Al–Mg–Si Alloys in a Wide Range of Heating Rates

In the present study, the dissolution and precipitation behaviour of four different aluminium alloys (EN AW-6005A, EN AW-6082, EN AW-6016, and EN AW-6181) in four different initial heat treatment conditions (T4, T6, overaged, and soft annealed) was investigated during heating in a wide dynamic range. Differential scanning calorimetry (DSC) was used to record heating curves between 20 and 600 °C. Heating rates were studied from 0.01 K/s to 5 K/s. We paid particular attention to control baseline stability, generating flat baselines and allowing accurate quantitative evaluation of the resulting DSC curves. As the heating rate increases, the individual dissolution and precipitation reactions shift to higher temperatures. The reactions during heating are significantly superimposed and partially run simultaneously. In addition, precipitation and dissolution reactions are increasingly suppressed as the heating rate increases, whereby exothermic precipitation reactions are suppressed earlier than endothermic dissolution reactions. Integrating the heating curves allowed the enthalpy levels of the different initial microstructural conditions to be quantified. Referring to time–temperature–austenitisation diagrams for steels, continuous heating dissolution diagrams for aluminium alloys were constructed to summarise the results in graphical form. These diagrams may support process optimisation in heat treatment shops.

Continuous cooling precipitation diagram of high alloyed Al-Zn-Mg-Cu 7049A alloy

Abstract The precipitation behaviour during cooling from solution annealing of high alloyed 7049A aluminium alloy was investigated, covering the complete cooling-rate-range of technical interest. This ranges from slow cooling rates close to equilibrium up to rates above complete supersaturation and is covering seven orders of magnitude in cooling rate (0.0005 to 5000 K/s). The continuous cooling precipitation behaviour of 7049A alloy was recorded by combining different differential scanning calorimetry (DSC) techniques and microstructure analysis by SEM and Vickers hardness testing. The high alloyed, high strength and quench sensitive wrought aluminium alloy 7049A was investigated during quenching from solution annealing by conventional DSC in the cooling rate range of 0.0005 to 4 K/s. In this range at least two exothermal precipitation reactions were observed: a high temperature reaction in a narrow temperature interval of 450–430 °C, and a low temperature reaction in a broad temperature interval down to about 200 °C. Intensities of both reactions decreased with increasing cooling rate. Quenching from solution annealing with rates up to 1000 K/s was investigated by differential fast scanning calorimetry (DFSC) and the differential reheating method (DRM). A critical quenching rate to suppress all precipitation reactions of 100–300 K/s was been determined.

Das kontinuierliche Zeit-Temperatur-Ausscheidungs-Diagramm einer Aluminiumlegierung EN AW-6005A*

Kurzfassung Der Einfluss der Abschreckgeschwindigkeit auf das Ausscheidungsverhalten von Aluminiumlegierungen wird, in Anlehnung an ZTU-Diagramme von Stählen, in kontinuierlichen Zeit-Temperatur-Ausscheidungs-Diagrammen dargestellt. Solche Diagramme sind bisher kaum verfügbar, können jetzt aber mit Hilfe der Differential Scanning Calorimetry (DSC) erfasst werden. Wird eine Charge der Aluminiumlegierung EN AW-6005A in einem Kühlgeschwindigkeitsbereich von 0,1–30 K/min von Lösungsglühbedingungen in einem DSC abgekühlt, sind in den Abkühlkurven zwei exotherme Ausscheidungsreaktionen zu erkennen, eine Hoch- sowie eine Niedertemperaturreaktion. Um Aufschluss darüber zu erhalten, welche Phasen dabei ausgeschieden werden, wurden umfangreiche Gefügeanalysen mittels Licht- und Rasterelektronenmikroskopie, energiedispersiver Röntgen-Mikroanalyse (EDX), Röntgendiffraktometrie (XRD) und Elektronen-Rückstreubeugung (EBSD) sowie Härteprüfungen an unterschiedlich abgekühlten Proben durchgeführt. Es konnte gezeigt werden, dass bei der Hochtemperaturreaktion Mg2Si ausgeschieden wird. Die Keimbildung der Mg2Si-Partikel erfolgt überwiegend heterogen an Primärausscheidungen.

Precipitation of a new platelet phase during the quenching of an Al-Zn-Mg-Cu alloy

A previously undescribed high aspect ratio strengthening platelet phase, herein named the Y-phase, has been identified in a commercial Al-Zn-Mg-Cu alloy. Differential scanning calorimetry indicates that this phase only precipitates at temperature and cooling rate of about 150–250 °C and 0.05–300 K/s, respectively. This precipitate is shown to be responsible for a noticeable improvement in mechanical properties. Aberration corrected scanning transmission electron microscopy demonstrates the minimal thickness (~1.4 nm) precipitate plates are isostructural to those of the T1 (Al2CuLi) phase observed in Al-Cu-Li alloys. Low voltage chemical analysis by energy dispersive X-ray spectroscopy and electron energy loss spectroscopy gives evidence of the spatial partitioning of the Al, Cu and Zn within the Y-phase, as well as demonstrating the incorporation of a small amount of Mg.

Continuous cooling precipitation diagram of cast aluminium alloy Al-7Si-0.3Mg

Abstract The precipitation behaviour during quenching of cast Al-7Si-0.3Mg aluminium alloy was investigated by DSC in the cooling rate range of 0.01 K/s to 3 K/s and by quenching dilatometry for higher rates. Two main precipitation reactions were observed during cooling, a high temperature reaction starting almost directly with quenching from 540 °C and a low temperature reaction starting at about 400 °C. Quenching with 3 K/s already significantly suppresses precipitation during quenching. Hardness after T6 ageing increases with increasing quenching rate, due to the increasing content of supersaturated solid solution. By dilatometry and hardness results the critical cooling rate can be estimated as about 60 K/s. Quenched Al-7Si-0.3Mg microstructures have been investigated by light microscopy. The microstructures consist of an aluminium–silicon eutectic structure, aluminium solid solution dendrites and precipitates inside the aluminium dendrites, depending on quenching rate.

Isothermal Time-Temperature-Precipitation Diagram for an Aluminum Alloy 6005A by In Situ DSC Experiments

Time-temperature-precipitation (TTP) diagrams deliver important material data, such as temperature and time ranges critical for precipitation during the quenching step of the age hardening procedure. Although the quenching step is continuous, isothermal TTP diagrams are often applied. Together with a so-called Quench Factor Analysis, they can be used to describe very different cooling paths. Typically, these diagrams are constructed based on mechanical properties or microstructures after an interrupted quenching, i.e., ex situ analyses. In recent years, an in situ calorimetric method to record continuous cooling precipitation diagrams of aluminum alloys has been developed to the application level by our group. This method has now been transferred to isothermal experiments, in which the whole heat treatment cycle was performed in a differential scanning calorimeter. The Al-Mg-Si-wrought alloy 6005A was investigated. Solution annealing at 540 °C and overcritical quenching to several temperatures between 450 °C and 250 °C were followed by isothermal soaking. Based on the heat flow curves during isothermal soaking, TTP diagrams were determined. An appropriate evaluation method has been developed. It was found that three different precipitation reactions in characteristic temperature intervals exist. Some of the low temperature reactions are not accessible in continuous cooling experiments and require isothermal studies.

Correlation between Supersaturation of Solid Solution and Mechanical Behaviour of Two Binary Al-Si-Alloys

Cooling of age-hardening Al-alloys after solution annealing is a critical step with respect to distortion and residual stresses. In order to predict their extent by simulation models, the mechanical behaviour must be known in a wide range of conditions and compositions. Therefore, experimental data is needed both for calibration and validation of the mechanical model. It is known for Al-Mg-Si alloys that supersaturation of the solid solution leads to a significant increase of strength during cooling. In order to understand the influence of single alloying elements on the strengthening effect, the mechanical properties of different binary alloys are investigated experimentally. The precipitation behaviour during cooling was investigated by Differential Scanning Calorimetry in a wide cooling rate range. A methodology to determine the degree of supersaturation of the solid solution based on the calorimetric results is presented. This approach is compared to atom probe tomography data. The mechanical behaviour of the alloys after various heat treatments was analysed by mechanical tests performed in a quenching and deformation dilatometer. Flow curves with high resolution at small strains (< 3 %) were measured at different temperatures. The results of the different experimental techniques are discussed in comparison and with respect to their testing limitations.

Short-time heat treatment of press hardened steel for laser assisted clinching

Abstract Clinching of high strength steels is currently difficult due to their relative low ductility. Hence a new method has been developed to clinch these steel grades. This could be achieved by heating the sheets locally at the joint by a laser during the clinching process. The short-time tempering behaviour of the press hardened steel 22MnB5 has been investigated by dilatometry respectively calorimetry experiments. Different stages of the tempering process have been identified depending on heating rates up to 1000 K s−1. Characteristic tempering reactions were shifted to higher temperatures with increasing heating rate. Based on these results, suitable short-time heat treatment parameters have been selected and transferred to the clinching process. Thereby the press hardened steel 22MnB5 has been successfully clinched with laser assistance for the very first time. The laser assisted clinched joint has been characterised by metallographic analysis and hardness testing. It could be shown, that in the clinching joint only a slight strength loss occurs due to the introduced laser heat.

Detection of Quench Induced Precipitation in Al Alloys by Dilatometry

Quenching is a critical step during the strengthening age hardening of Aluminium alloys. To obtain optimal technological results, parts should be quenched with the upper critical cooling rate. The precipitation behaviour of Al alloys during cooling from solution annealing and thereby the critical cooling rates are typically investigated by in-situ measurements with differential scanning calorimetry (DSC). Conventional DSCs are limited at cooling rates below 10 Ks-1. Unfortunately, medium to high strength Al alloys typically have critical cooling rates between 10 and some 100 Ks-1. Recently it was shown that dilatometry is generally able for in-situ detection of precipitation in Al alloys. Dilatometry allows controlled cooling up to some 100 Ks-1 and therefore covers the cooling rate range relevant. In this work, we aim to show up and discuss possibilities and limitations of dilatometric detection of quench induced precipitates in 2xxx, and 7xxx Al alloys. The basic method will be presented and results will be compared with DSC work.

Precipitation Behaviour and Mechanical Properties during Short-Term Heat Treatment for Tailor Heat Treated Profiles (THTP) of Aluminium Alloy 6060 T4

Precipitation hardening aluminium alloys are widely used for automotive applications. To enhance the application of aluminium profiles, improved formability is needed. Tailor Heat Treated Profiles (THTP) with locally different material properties attempt to increase formability e.g. in bending processes. Tailoring of local properties is obtained by a local short-term heat treatment, dissolving the initial precipitate state (retrogression) and still allowing subsequent ageing. In the present study, the dissolution and precipitation behaviour of the aluminium alloy EN AW-6060 T4 was investigated during heating with differential scanning calorimetry (DSC). Heating curves from 20 to 600 °C with heating rates of 0.01 up to 5 K/s were recorded. Interrupted heat treatments with different maximum temperatures were performed in a deformation dilatometer. Immediately afterwards, tensile tests were carried out at room temperature. The course of the recorded mechanical properties as a function of the maximum temperature is discussed with regard to the dissolution and precipitation behaviour during heating. Finally, the aging behaviour of the investigated alloy was recorded after different typical short-term heat treatments and is discussed with reference to the DSC‐curves. The correlation of the microstructure and the mechanical properties enables the derivation of optimal parameters for the development of THTP through a local softening.