Requirements for Processing High-Strength AlZnMgCu Alloys with PBF-LB/M to Achieve Crack-Free and Dense Parts.

Processing aluminum alloys employing powder bed fusion of metals (PBF-LB/M) is becoming more attractive for the industry, especially if lightweight applications are needed. Unfortunately, high-strength aluminum alloys such as AA7075 are prone to hot cracking during PBF-LB/M, as well as welding. Both a large solidification range promoted by the alloying elements zinc and copper and a high thermal gradient accompanied with the manufacturing process conditions lead to or favor hot cracking. In the present study, a simple method for modifying the powder surface with titanium carbide nanoparticles (NPs) as a nucleating agent is aimed. The effect on the microstructure with different amounts of the nucleating agent is shown. For the aluminum alloy 7075 with 2.5 ma% titanium carbide nanoparticles, manufactured via PBF-LB/M, crack-free samples with a refined microstructure having no discernible melt pool boundaries and columnar grains are observed. After using a two-step ageing heat treatment, ultimate tensile strengths up to 465 MPa and an 8.9% elongation at break are achieved. Furthermore, it is demonstrated that not all nanoparticles used remain in the melt pool during PBF-LB/M.

Nucleation Behavior of a Single Al-20Si Particle Rapidly Solidified in a Fast Scanning Calorimeter.

Understanding the rapid solidification behavior characteristics, nucleation undercooling, and nucleation mechanism is important for modifying the microstructures and properties of metal alloys. In order to investigate the rapid solidification behavior in-situ, accurate measurements of nucleation undercooling and cooling rate are required in most rapid solidification processes, e.g., in additive manufacturing (AM). In this study, differential fast scanning calorimetry (DFSC) was applied to investigate the nucleation kinetics in a single micro-sized Al-20Si (mass%) particle under a controlled cooling rate of 5000 K/s. The nucleation rates of primary Si and secondary α-Al phases were calculated by a statistical analysis of 300 identical melting/solidification experiments. Applying a model based on the classical nucleation theory (CNT) together with available thermodynamic data, two different heterogeneous nucleation mechanisms of primary Si and secondary α-Al were proposed, i.e., surface heterogeneous nucleation for primary Si and interface heterogenous nucleation for secondary α-Al. The present study introduces a practical method for a detailed investigation of rapid solidification behavior of metal particles to distinguish surface and interface nucleation.

In-situ analysis of continuous cooling precipitation in Al alloys by wide-angle X-ray scattering.

The aim of this work is to investigate quench induced precipitation during continuous cooling in aluminium wrought alloys EN AW-7150 and EN AW-6082 using in situ synchrotron wide-angle X-ray scattering (WAXS). While X-ray diffraction is usually an ex situ method, a variety of diffraction patterns were recorded during the cooling process, allowing in situ analysis of the precipitation process. The high beam energy of about 100 keV allows the beam to penetrate a bulk sample with a 4 mm diameter in a quenching dilatometer. Additionally, the high intensity of a synchrotron source enables sufficiently high time resolution for fast in situ cooling experiments. Reaction peaks could be detected and compared with results from differential scanning calorimetry (DSC) by this method. A methodology is presented in this paper to evaluate WAXS data in a way that is directly comparable to DSC-experiments. The results show a high correlation between both techniques, DSC and WAXS, and can significantly improve continuous cooling precipitation diagrams.

Development of Precipitation Hardening Parameters for High Strength Alloy AA 7068.

The mechanical properties after age hardening heat treatment and the kinetics of related phase transformations of high strength AlZnMgCu alloy AA 7068 were investigated. The experimental work includes differential scanning calorimetry (DSC), differential fast scanning calorimetry (DFSC), sophisticated differential dilatometry (DIL), scanning electron microscopy (SEM), as well as hardness and tensile tests. For the kinetic analysis of quench induced precipitation by dilatometry new metrological methods and evaluation procedures were established. Using DSC, dissolution behaviour during heating to solution annealing temperature was investigated. These experiments allowed for identification of the appropriate temperature and duration for the solution heat treatment. Continuous cooling experiments in DSC, DFSC, and DIL determined the kinetics of quench induced precipitation. DSC and DIL revealed several overlapping precipitation reactions. The critical cooling rate for a complete supersaturation of the solid solution has been identified to be 600 to 800 K/s. At slightly subcritical cooling rates quench induced precipitation results in a direct hardening effect resulting in a technological critical cooling rate of about 100 K/s, i.e., the hardness after ageing reaches a saturation level for cooling rates faster than 100 K/s. Maximum yield strength of above 600 MPa and tensile strength of up to 650 MPa were attained.

Review of the Quench Sensitivity of Aluminium Alloys: Analysis of the Kinetics and Nature of Quench-Induced Precipitation.

For aluminium alloys, precipitation strengthening is controlled by age-hardening heat treatments, including solution treatment, quenching, and ageing. In terms of technological applications, quenching is considered a critical step, because detrimental quench-induced precipitation must be avoided to exploit the full age-hardening potential of the alloy. The alloy therefore needs to be quenched faster than a critical cooling rate, but slow enough to avoid undesired distortion and residual stresses. These contrary requirements for quenching can only be aligned based on detailed knowledge of the kinetics of quench-induced precipitation. Until the beginning of the 21st century, the kinetics of relevant solid-solid phase transformations in aluminium alloys could only be estimated by ex-situ testing of different properties. Over the past ten years, significant progress has been achieved in this field of materials science, enabled by the development of highly sensitive differential scanning calorimetry (DSC) techniques. This review presents a comprehensive report on the solid-solid phase transformation kinetics in Al alloys covering precipitation and dissolution reactions during heating from different initial states, dissolution during solution annealing and to a vast extent quench-induced precipitation during continuous cooling over a dynamic cooling rate range of ten orders of magnitude. The kinetic analyses are complemented by sophisticated micro- and nano-structural analyses and continuous cooling precipitation (CCP) diagrams are derived. The measurement of enthalpies released by quench-induced precipitation as a function of the cooling rate also enables predictions of the quench sensitivities of Al alloys using physically-based models. Various alloys are compared, and general aspects of quench-induced precipitation in Al alloys are derived.

Scanning Rate Extension of Conventional DSCs through Indirect Measurements.

In this work, a method is presented which allows the determination of calorimetric information, and thus, information about the precipitation and dissolution behavior of aluminum alloys during heating rates that could not be previously measured. Differential scanning calorimetry (DSC) is an established method for in-situ recording of dissolution and precipitation reactions in various aluminum alloys. Diverse types of DSC devices are suitable for different ranges of scanning rates. A combination of the various available commercial devices enables heating and cooling rates from 10-4 to 5 Ks-1 to be covered. However, in some manufacturing steps of aluminum alloys, heating rates up to several 100 Ks-1 are important. Currently, conventional DSC cannot achieve these high heating rates and they are still too slow for the chip-sensor based fast scanning calorimetry. In order to fill the gap, an indirect measurement method has been developed, which allows the determination of qualitative information, regarding the precipitation state, at various points of any heat treatment. Different rapid heat treatments were carried out on samples of an alloy EN AW-6082 in a quenching dilatometer and terminated at defined temperatures. Subsequent reheating of the samples in the DSC enables analysis of the precipitation state of the heat-treated samples. This method allows for previously un-measurable heat treatments to get information about the occurring precipitation and dissolution reactions during short-term heat treatments.

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.

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.