The present dissertation reports the findings of a study of cracking behavior of a newly developed superalloy, Allvac 718Plus during high power beam welding and post-weld heat treatment. Microstructures of the base alloy, heat affected zone (HAZ) and fusion zone (FZ) of welded and post-weld heat treated (PWHT) coupons were examined by the use of standard metallographic techniques involving optical microscopy, analytical scanning electron microscopy (SEM) and analytical transmission electron microscopy. Moreover, grain boundary segregation behavior of boron atoms during pre-weld heat treatments was evaluated using secondary ion mass spectroscopic system. In the first phase of the research, 718Plus was welded using a low and high heat input CO2 laser to assess its weld cracking response. Detailed examination of the welds by analytical electron microscopic technique revealed the occurrence of cracking in the HAZ of low heat input welds, while their FZ was crack free. However, both the FZ and HAZ of high heat input welds were crack-free. Resolidified constituents were observed along the cracked grain boundaries of the lower heat input welds, which indicated that HAZ cracking in this newly developed superalloy was associated with grain boundary liquation. However, despite a more extensive liquation of grain boundaries and grain interior in the HAZ of high heat input welds, no cracking occurred. This was attributed to the combination of lower welding stresses generated during cooling, and relaxation of these stresses by thick intergranular liquid. Although HAZ cracking was prevented by welding with a high heat input laser, it resulted in a significant damage to the parent microstructure through its extensive liquation. Thus, the use of low heat input welding is desirable. However, this resulted in HAZ cracking which needs to be minimized or eliminated. Therefore, during the second phase of this research, the effects of pre-weld thermal processing on the cracking response of 718Plus were investigated. Results from the quantification of the cracking of the alloy showed that HAZ cracking may be significantly reduced or eliminated through an adequate selection of pre-weld thermal cycle. In the third stage of this research, crack-free welds of 718Plus were post-weld heat treated using standard thermal schedules. A significant solid state cracking of the alloy occurred during the PWHT. The cracking was attributed to the presence of embrittling phases on HAZ grain boundaries, coupled with aging contraction stresses that are generated by a considerable precipitation of gamma prime phase during aging.

[pt] A presente tese tem como objetivo estudar a estabilidade microestrutural da superliga 625 a base de Ni pelas suas propriedades mecânicas e suas várias aplicações na indústria, em três condições distintas: maciça (placa forjada industrialmente), partículas de pó precursora da peça 3D e uma peça produzida por impressão a laser (Deposição Direta de Metais - DMD). Amostras destas condições foram submetidas a tratamentos de solubilização e envelhecimento isotérmico a 650 graus Celsius e 750 graus Celsius durante 10 horas e 100 horas, de modo a promover fenômeno de precipitação e, assim, correlacionar com as propriedades mecânicas do material. A caracterização microestrutural foi realizada por microscopia ótica (MO), microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET) no modo convencional utilizando contraste de difração, na modalidade analítica de transmissão/varredura (STEM), e em alta resolução (HRTEM). Espectroscopias de raios X por dispersão em energia (EDS) e de perdas de energia de elétrons (EELS) foram utilizadas para analisar a composição local da matriz e das fases presentes. Foram realizados ensaios de microdureza para avaliar o efeito dos tratamentos térmicos. A análise microestrutural da amostra maciça na condição como recebida apresentou grãos equiaxiais com fases NbTiC e M6C. Com o tratamento térmico de solubilização a 1100 graus Celsius por 40 minutos houve uma dissolução parcial dos carbetos. O envelhecimento a 650 graus Celsius por 10 horas resultou em carbetos de NbTiC e um aumento da dureza em 5 porcento em relação a amostra como solubilizada. Entretanto no tratamento de envelhecimento a 100 horas ocorreu precipitação homogênea da fase gama aumentando a dureza do material em 45 porcento, se comparada à mesma como solubilizada. A liga maciça envelhecida a 750 graus Celsius por 10 horas apresentou os carbetos NbTiC e M23C6 nos contornos de grãos e dispersos na matriz. Já a liga maciça envelhecida por 100 horas a esta mesma temperatura, apresentou a fase δ dispersa na matriz. A análise microestrutural do pó precursor mostrou ser policristalino constituído predominantemente de grãos colunares da matriz austenítica. Análises das amostras produzidas por DMD como recebida revelou estrutura dendrítica com carbetos de Nb e fase Laves nas regiões interdendríticas. A solubilização das amostras DMD durante 40 minutos por 1100 graus Celsius e 1200 graus Celsius mostrou ser insuficientes para a dissolução dos precipitados. A fim de melhorar a difusão do Nb e a dissolução dos carbetos e da fase Laves, foi realizado o tratamento de solubilização a 1200 graus Celsius por 100 horas. Esta amostra tratada a 650 graus Celsius por 100 horas apresentou carbetos M23C6 precipitados nos contornos de grão e nas interfaces entre matriz CFC e a fase Laves. Entretanto, no envelhecimento a 750 graus Celsius durante 100 horas ocorreu à precipitação dos carbetos M23C6 e M6C nos contornos de grão e dispersos na matriz, aumentando assim a dureza do material em 18 porcento, se comparada à mesma como solubilizada. O aumento da microdureza em 12 porcento após o tratamento térmico está relacionado à precipitação dos carbetos nos contornos de grão e dispersos na matriz resultado dos tratamentos térmicos de envelhecimento. / [en] This thesis studies the microstructural stability of Ni-base Super alloy 625 for its mechanical properties and its varieties of applications in the industry, in three different conditions: bulk (industrially forged plate), precursor powder particles for 3D printing process and a sample produced by laser Direct Metal Deposition (DMD). Aiming at promoting precipitation processes and, therefore, correlate with the mechanical properties of the material, samples of these conditions were submitted to solution annealing and isothermal aging treatments at 650 Celsius degrees and 750 Celsius degrees for 10 hours and 100 hours. Characterization of the microstructure was performed by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), in the conventional diffraction contrast mode, scanning/transmission (STEM) analytical mode, and high resolution microscopy (HRTEM). Energy dispersive X-ray spectrometry (EDXS) and electron energy loss spectroscopy (EELS) were used to analyze the local composition of the matrix and precipitated phases. Micro hardness measurements were performed to evaluate the effect of thermal treatments. The microstructural analysis of the bulk sample in the as-received condition showed an equiaxial grain structure with NbTiC and M6C precipitated phases. Solid solution treatment at 1100 Celsius degrees for 40 minutes allowed partial dissolution of the carbides. Aging at 650 Celsius degrees for 10 hours showed NbTiC carbides and a hardness increase of 5 percent compared to the as-solubilized sample. However, aging at this temperature for 100 hours promoted the homogeneous precipitation of the gama phase, thus increasing the material s hardness by 45 percent, when compared to it as solubilized. The bulk sample aged at 750 Celsius degrees for 10 hours showed grain boundary and homogeneous precipitation of NbTiC and M23C6 carbides. This sample condition upon aging at this temperature for 100 hours shows δ phase homogeneously precipitated in the matrix. The microstructural analysis of the precursor powder showed micrometer size individual particles as polycrystalline, consisting predominantly of columnar grains of the austenitic matrix. Analysis of samples produced by DMD in the as-received condition revealed dendritic microstructure with carbides of Nb and Laves phase in the interdendritic regions. The solution treatment of the DMD samples for 40 minutes at 1100 Celsius degrees and 1200 Celsius degrees proved to be insufficient for the dissolution of the precipitate. In order to enhance diffusion of Nb and so carbide and Laves phase dissolution, a solution anneal was carried out at 1200 Celsius degrees for 100 hours. This sample treated at 650 Celsius degrees for 100 hours showed M23C6 carbides precipitated at grain boundaries and also at the Laves phase/matrix interfaces. However, upon aging at 750 Celsius degrees for 100 hours the precipitation of M23C6 and M6C takes place at the grain boundary and in the austenitic matrix, thus increasing the material s hardness by 18 percent, when compared to it as solubilized. The increase of the hardness by 12 percent after the heat treatment is related to the precipitation of the carbides in the grain boundaries and dispersed in the matrix resulting from the aging thermal treatments.