Precipitation (chemistry)

Summary

In an aqueous solution, precipitation is the process of transforming a dissolved substance into an insoluble solid from a supersaturated solution. The solid formed is called the precipitate. In case of an inorganic chemical reaction leading to precipitation, the chemical reagent causing the solid to form is called the precipitant. The clear liquid remaining above the precipitated or the centrifuged solid phase is also called the supernate or supernatant. The notion of precipitation can also be extended to other domains of chemistry (organic chemistry and biochemistry) and even be applied to the solid phases (e.g. metallurgy and alloys) when solid impurities segregate from a solid phase. Supersaturation The precipitation of a compound may occur when its concentration exceeds its solubility. This can be due to temperature changes, solvent evaporation, or by mixing solvents. Precipitation occurs more rapidly from a strongly supersaturated solution. The formation of a preci

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The aim of the thesis is to obtain more understanding about the influence of plastic deformation on the microstructural changes observed in single crystal (SX) Ni-based superalloys using diffraction techniques. This work was organised around two main problematics: (1) rafting in turbine blades after the manufacturing process and (2) rafting and mosaicity evolution in two SX alloys with different composition during creep deformation. SX Ni-based superalloys are first choice materials for turbine blade application in land-based gas turbines and aero-engines. Superior mechanical properties of these materials at high temperatures are achieved due to the optimisation of the alloying composition and the microstructure. SX Ni-based superalloy turbine blades solidify by dendritic solidification with dendrites aligned along the directions of lowest Young modulus (interdendritic spacing around 300μm). At the end of the manufacturing process, the microstructure consists of high volume fraction of cubic γ’ precipitates (around 500nm) coherently embedded in the γ matrix. However specific parts of engine-ready turbine blades exhibit directionally coarsened γ’ precipitates in a preferred direction (rafting) without the influence of an applied load. It is of prime importance to understand the origin of rafting prior to the introduction of the blades in the engine since rafting can alter the mechanical properties of the alloy. Chemical segregations and the introduction of plastic deformation prior to thermal treatments were identified as potential driving force for rafting during load-free high temperature annealing. Most of the SX Ni-based superalloys used in the current blade production in Alstom contain significant amount of refractory elements which are expensive and increase the density of the alloy. To answer the demand of cheaper and lighter components, Alstom launched a development program to design novel SX superalloys. One of these projects led to the production of a Re-free superalloy, so-called MD2. Extensive mechanical investigations on MD2 are on-going and compared to the behaviour of the MK4HC alloy (3wt% Re) currently used in turbine blade production. One of the major differences in terms of mechanical properties between Re-containing and Re-free SX alloys is the faster kinetics of coarsening and rafting during creep deformation at high temperature in the latter alloys. It prevented so far their application in the hottest areas in gas turbines. It is therefore of utmost importance to acquire more knowledge about the mechanisms associated with the microstructure evolution during creep of the new MD2 SX alloy in comparison with the MK4HC alloy. The evolution of the lattice parameter misfit in different directions with respect to the applied load during creep deformation was associated with the evolution of the microstructure from cubic to elongated γ’ precipitates It could be shown that rafting occurs after the cooling stage following the solution heat treatment (SHT) during the manufacturing of the blade with investigations of the microstructure. The influence of chemical segregations on rafting was excluded with the investigation of the blade alloy composition in different parts of the blade cooled from the SHT and diffraction measurements in stress-relieved combs prepared from the same blade. The formation of a rafted microstructure during the manufacturing process was associated with the formation of plastic strains during cooling after the SHT. This was confirmed after gathering results from investigations of the microstructure, simulation of the cooling stage and neutron diffraction measurements on the blade. The investigations of the microstructure performed on the engine-ready blade revealed an inversion of the γ’ raft orientation below (parallel to [001]) and above the platform of the blade (perpendicular to [001]). This was attributed to an inversion of the sign of residual strain between the previously mentioned positions as revealed by neutron diffraction measurements performed along the airfoil of the blade cooled after the SHT. Microscopy also showed that the rafted microstructure was more pronounced below the platform (long γ’ rafts) than above the platform (shorter γ’ rafts with retained cubic precipitates). The concept of the threshold plastic strain necessary to induce rafting during annealing subsequent to plastic deformation was used to describe the difference in rafted microstructure. It is suggested that plastic strains largely exceed the threshold below the platform leading to fully formed rafted microstructure. On the other side, plastic strains of the order to the threshold strain are suggested above the platform in order to explain the partially formed rafted microstructure Neutron diffraction measurements revealed that the lattice parameter misfit was larger in the MK4HC than in the MD2 alloy at 20°C in the unloaded state. The larger misfit in the MK4HC alloy was attributed to the larger concentration of elements dissolving in the γ phase and to the presence of Re. During creep deformation, coherency stresses are relieved at the γ/γ’ interface in the γ channels perpendicular to the applied load by dislocations. On the other hand, dislocations increase the internal stress at the γ/γ’ interface in the γ channels parallel to the applied load. This leads to the rafting of the γ’ precipitates perpendicular to the applied load. This was observed in the MK4HC. The absence of clear misfit evolution in the MD2 alloy was attributed to the anomalous microstructure at the beginning of the creep deformation. The mosaicity of the MK4HC and MD2 alloys revealed crystallographic misorientation between neighbouring dendrites up to 0.5°. The misorientation was associated with the presence of dislocations in the regions between the dendrites formed during the dendritic solidification of the alloys from existing work. It was shown that the composition of the SX alloys and short periods at high temperature in the unloaded state had only little influence on the misorientation between neighbouring dendrites. Upon creep loading to 180MPa, the mosaicity markedly changed in the two SX alloys independent of the creep temperature. In particular, the number of single misoriented domains measured by X-ray diffraction decreased. This was attributed to the fast propagation of the dislocations present in the interdendritic structure inducing a rotation of the individual dendrites. During creep deformation, the mosaicity increased as visible from the broadening of the maximum spread in misorientation. The formation of inhomogeneous plastic strain fields in the γ/γ’ microstructure is believed to create new mosaic blocks in the dendritic structure of the alloys leading to the observed broadening of the mosaicity. The influence of plastic deformation on the evolution of the mosaicity was demonstrated. The mosaicity significantly changed during creep of the MD2 at 1050°C/180MPa and 1000°C/180MPa whereas no significant evolution could be measured during creep at 950°C/180MPa. This was attributed to a temperature dependence of the yield strength of the MD2 alloy. It therefore induces difference in dislocation propagation at 950°C compared to 1050°C and 1000°C which retards the broadening of the mosaicity during creep at 950°C. Furthermore, the mosaicity formed during creep deformation was retained upon unloading and cooling of the SX samples to room temperature.

EPFL2012

Additive Manufacturing of L12 Precipitate Strengthened Nickel and Aluminum Alloys

Seth James Griffiths

Metal Additive Manufacturing (AM) technologies have enabled the manufacturing of parts with complex geometries that were previously not feasible with conventional manufacturing. Unfortunately, many commercial engineering alloys (with the exception of alloys for welding) were designed with conventional manufacturing in mind and can behave poorly in the rapid solidification and thermal conditions that go along with AM. Research is needed to optimize the higher performance engineering alloys, such as pre-cipitation hardened alloys, for AM. One important class of precipitates in both the nick-el-base and aluminum-base superalloys is the intermetallic L12 âstructured (Strukturbericht notation) intermetallics. Many scientific challenges must be overcome prior to widespread industrial usage of these alloys. AM of L12-strengthened Ni-base superalloys results in extensive micro-cracking and AM of L12-strengthened Al-base alloys has been successful but requires further research to understand the material be-havior. This thesis focuses on overcoming the scientific challenges for the AM of L12-strengthened alloys. A new Al-Mg-Zr alloy strengthened via L12-structured Al3Zr precipitates, AddalloyÂ®,was successfully fabricated for the first time with Laser-Powder Bed Fusion (L-PPF). The as-fabricated Al-Mg-Zr alloy displayed a unique bimodal grain structure: (i) the bottom of the melt pools consisted of fine equiaxed grains (~1 Âµm) and (ii) the top of the melt pool consisted of columnar grains (up to 40 Âµm long). The bimodal microstructure was at-tributed to the changing solidification conditions during the lifetime of the melt. A new microstructure modification strategy, laser rescanning, was shown to refine the micro-structure. The grain refinement was attributed to the reduced melt pool depths of the additional scans, thus breaking up the previously solidified columnar grains. Scanning transmission electron microscopy (STEM) investigations of peak-aged (400ËC, 8 h) samples reveal both continuous (~2 nm in diameter) and discontinuous (~5 nm wide and hundreds of nanometers long) coherent, secondary L12-Al3Zr precipitates. The Al-Mg-Zr in the peak aged (400ËC, 8 h) condition had a 385 MPa yield strength and a 19% elongation at fracture. The excellent combination of strength and ductility was attribut-ed to the bimodal microstructure. For short-term elevated temperature yield tests, as-fabricated samples displayed higher yield strengths than peak-aged samples at temper-atures above 150ËC (e.g., 87 vs 24 MPa at 260ËC). For longer term creep tests at 260 ËC, both as-fabricated and peak-aged samples displayed near-identical creep behavior. The reduced elevated temperature performance of the peak aged samples was attributed to coarsening of grain-boundary precipitates during aging, decreasing their ability to in-hibit grain-boundary sliding (GBS) of the fine equiaxed grains. The micro-cracking of CM24LC, a Ni-base superalloy, was attributed to both solidifica-tion and liquation cracking. Based on experimental evidence, reduction in the solidifica-tion interval of CM247LC was investigated as a candidate for micro-crack mitigation and a new alloy was developed. As Hf is found to have a significant influence on the freezing range of the alloy, a new CM247LC without Hf was produced and tested. Sam-ples fabricated with the Hf-free CM247LC, CM247LC NHf, in combination with opti-mized processing conditions exhibit a reduction in crack density of 98%.

EPFL2020

Development of High-Strength Aluminum Alloys for Additive Manufacturing

Marvin Lennard Schuster

Metal additive manufacturing (AM) offers the possibility to rapidly produce complex geometries that are not achievable with conventional manufacturing methods. The two most common technologies, Laser Powder Bed Fusion (LPBF) and Direct Metal Deposition (DMD), are characterized by high process temperatures, fast heating, and cooling rates, and an associated far-from-equilibrium solidification. This is problematic when processing materials that were developed and optimized many years ago for conventional manufacturing processes. Common difficulties are the occurrence of gas pores in the component, which are caused by the evaporation of volatile alloying elements during the process, the formation of hot cracks due to large solidification intervals, and the formation of metastable phases. For the processing of high-strength, precipitation-hardening Al-Cu aluminum alloys, this prevents the use of non-modified conventional alloys. However, the development of novel alloys tailored to these processes not only allows these difficulties to be overcome but also opens up the possibility of improving material properties through the targeted exploitation of process-inherent properties. This includes the processing of oxide particle-reinforced alloys, which can not be produced by conventional casting processes. The standard heat treatment usually performed for precipitation hardening, which has also been optimized for conventional materials, must be adapted accordingly to achieve optimum material properties. Within the scope of this work, the microstructure, precipitation, and defect formation after LPBF as well as the heat treatment behavior are thoroughly investigated based on an Al-Cu-Mg-Zr alloy for the first time. The obtained findings are applied to design a novel 2618 Al-Cu alloy for LPBF and DMD, with suitable heat treatment being developed for LPBF. The alloy is characterized with respect to microstructure, precipitation formation, and mechanical properties before, during, and after heat treatment. Furthermore, by modifying elemental Al-Zr powder blends with nm-sized Al2O3, an oxide dispersion strengthened alloy is produced by LPBF and investigated in detail.

EPFL2022