Process Gas Infiltration in Inconel 718 Samples during SLM Processing

Argon infiltration is a well-known problem of hot isostatic pressed components. Thus, the argon content is one quality attribute which is measured after a hot isostatic pressing (HIP) process. Since the Selective Laser Melting (SLM) process takes place under an inert argon atmosphere; it is imaginable that argon is entrapped in the component after SLM processing. Despite using optimized process parameters, defects like pores and shrink holes cannot be completely avoided. Especially, pores could be filled with process gas during the building process. Argon filled pores would clearly affect the mechanical properties. The present paper takes a closer look at the porosity in Inconel 718 samples, which were generated by means of SLM. Furthermore, the argon content of the powder feedstock, of samples made by means of SLM, of samples which were hot isostatic pressed after the SLM process, and of conventionally manufactured samples were measured and compared. The results showed an increased argon content in the Inconel 718 samples after SLM processing compared to conventional manufactured samples.

The effect of dissolved magnesium on diffusion creep in calcite

We experimentally tested a series of synthetic calcite marbles with varying amounts of dissolved magnesium in a standard triaxial deformation machine at 300 MPa confining pressure, temperatures between 700 and 850°C, stresses between 2 and 100 MPa, and strain rates between 10−7 and 10−3 s−1. The samples were fabricated by hot isostatic pressing of a mixture of calcite and dolomite at 850°C and 300 MPa. The fabrication protocol resulted in a homogeneous, fine-grained high-magnesian calcite aggregate with minimal porosity and with magnesium contents between 0.07 and 0.17 mol% MgCO3. At stresses below 40 MPa the samples deformed with linear viscosity that depended inversely on grain size to the 3.26±0.51 power, suggesting that the mechanisms of deformation were some combination of grain boundary diffusion and grain boundary sliding. Because small grain sizes tended to occur in the high-magnesium calcite, the strength also appeared to vary inversely with magnesium content. However, the strength at constant grain size does not depend on the amount of dissolved magnesium, and thus, the impurity effect seems to be indirect. At stresses higher than 40 MPa, the aggregates become non-linearly viscous, a regime we interpret to be dislocation creep. The transition between the two regimes depends on grain size, as expected. The activation energy for diffusion creep is 200±30 kJ/mol and is quite similar to previous measurements in natural and synthetic marbles deformed at similar conditions with no added magnesium.

alpha-SiAlON-SiC composites obtained by gas-pressure sintering and hot-pressing

The objective of this work was the obtaining in situ of alpha-SiAlON-SiC composite, using an alternative rare-earth oxide mixture, RE2O3, as sintering additive, by two different sintering processes. As sintering additive, 20 vol.% of AlN-RE2O3 in a molar ratio of 90: 10 was mixed to the alpha-Si3N4 powder. In the Si3N4-AlN-RE2O3 powder mixture, 0, 10, 15 and 20wt.% of SiC were added. The powder batches were milled, dried and compacted by cold isostatic pressing. Two different sintering processes were used: gas-pressure sintering at 1950 degrees C for 1 h under 1.5 MPa of N-2 atmosphere, or uniaxial hot-pressing at 1750 degrees C, for 30 min under pressure of 20 MPa. The sintered samples were characterized by X-ray diffraction, scanning electron microscopy and mechanical properties. XRD patterns indicate only alpha-SiAlON (alpha') and beta-SiC as crystalline phases. It was observed that the SiC addition did not influence the alpha-SiAlON formation, although the growth of elongated alpha'-grains is substantially decreased. The hot-pressed composites presented better mechanical properties, exhibiting fracture toughness of 5 MPa m(1/2) and hardness around 21.5 GPa. (c) 2007 Elsevier B.V. All rights reserved.

Flux Pinning Optimization of MgB(2) Bulk Samples Prepared Using High-Energy Ball Milling and Addition of TaB(2)

MgB(2) is considered to be an important conductor for applications. Optimizing flux pinning in these conductors can improve their critical currents. Doping can influence flux pinning efficiency and grain connectivity, and also affect the resistivity, upper critical field and critical temperature. This study was designed to attempt the doping of MgB(2) on the Mg sites with metal-diborides using high-energy ball milling. MgB(2) samples were prepared by milling pre-reacted MgB(2) and TaB(2) powders using a Spex 8000M mill with WC jars and balls in a nitrogen-filled glove box. The mixing concentration in (Mg(1-x)Ta(x))B(2) was up to x = 0.10. Samples were removed from the WC jars after milling times up to 4000 minutes and formed into pellets using cold isostatic pressing. The pellets were heat treated in a hot isostatic press (HIP) at 1000 degrees C under a pressure of 30 kpsi for 24 hours. The influence that milling time and TaB(2) addition had on the microstructure and the resulting superconducting properties of TaB(2)-added MgB(2) is discussed. Improvement J(c) of at high magnetic fields and of pinning could be obtained in milled samples with added TaB(2) The sample with added 5at.% TaB(2) and milled for 300 minutes showed values of J(c) similar to 7 x 10(5) A/cm(2) and F(p) similar to 14 GN/m(3) at 2T, 4.2 K. The milled and TaB(2)-mixed samples showed higher values of mu(0)H(irr) than the unmilled-unmixed sample.

Physicochemical analysis of Ti-Si-B powder aalloys

Titanium alloys of Ti-Si-B system were manufactured by blended elemental powder method using Ti, Si and B powders as starting materials. It was found that uniaxial and isostatic pressing followed by hot pressing at around 1000°C, for 20 minutes, provided good densification of such alloys. The physicochemical studies were performed by means of scanning electron microscopy, X-ray diffraction, atomic force microscopy and microindentation/wear tests. The investigations revealed a multiphase microstructure formed mainly by α-titanium, Ti6Si2B, Ti5Si3, TiB and Ti3Si phases. The phase transformations after pressureless sintering at 1200°C was also studied by X-ray diffraction for the Ti-18Si-6B composition. As stated in some other researches, these intermetallics in the α-titanium matrix provide high wear resistance and hardness, with the best wear rate of 0.2 mm3/N.m and the highest hardness of around 1300 HV. © (2012) Trans Tech Publications, Switzerland.

Desenvolvimento de um cerâmico Al2O3/TI(C,N) para uso em maquinação

O principal objetivo deste trabalho é preparar um cermeto do tipo Al2O3/Ti(C,N) com propriedades mecânicas adequadas à sua utilização na maquinação de materiais do tipo DIN ISO 513:K01-K10 e ISO H01-H10. De forma a incrementar a sinterabilidade do cermeto investigou-se o efeito da adição de dopantes metálicos, nomeadamente alumínio metálico (Al) e hidreto de titânio (TiH2) e o efeito da substituição da moagem convencional por moagem de alta energia. As variáveis das etapas principais de processamento, i.e., da moagem, prensagem e sinterização, foram selecionadas com trabalho realizado quer na Universidade de Aveiro quer na empresa Palbit. Foram preparadas três composições do cermeto Al2O3/Ti(C,N) com adições de 5%TiH2, 1%Al e 5%TiH21%Al através da moagem de alta energia. Os parâmetros de moagem, i.e. a velocidade de rotação, o rácio bolas/pó e o tempo de moagem foram otimizados para os seguintes valores: 350 rpm, 10:1 e 5 h, respetivamente. A utilização da moagem de alta energia permitiu uma redução do tamanho de partícula dos pós até aproximadamente 100 nm e a obtenção de uma boa uniformidade da distribuição das fases (Al2O3+Ti(C,N)). A etapa de conformação foi efetuada por prensagem uniaxial seguida de prensagem isostática. A avaliação da reatividade dos cermetos através de dilatometria em atmosfera de vácuo revelou que a densificação é maioritariamente realizada em estado sólido. A adição de apenas 1%Al é a menos efetiva para a densificação. Os cermetos foram sinterizados através de sinterização convencional em forno de vazio a 1650ºC e prensagem a quente (1650ºC com uma pressão uniaxial de 25 MPa). Os valores de densificação obtidos, aproximadamente 80% e 100%, respetivamente, indicam que a aplicação de pressão durante a sinterização é efetiva para atingir densificações elevadas nos compactos, compatíveis com as suas aplicações tecnológicas. As propriedades mecânicas de dureza e de tenacidade avaliadas nos três cermetos apresentaram valores aproximados de 1800-1900 HV50 para a dureza e entre 5.4 e 7.7 MPa.m1/2 para a tenacidade à fratura.

Manufacture of ceramic membranes for application in demulsification process for cross-flow microfiltration

This paper describes the manufacture of tubular ceramic membranes and the study of their performance in the demulsification of soybean oil/water emulsions. The membranes were made by iso-static pressing method and micro and macro structurally characterized by SEM, porosimetry by mercury intrusion and determination of apparent density and porosity. The microfiltration tests were realized on an experimental workbench, and fluid dynamic parameters, such as transmembrane flux and pressure were used to evaluate the process relative to the oil phase concentration (analysed by TOC measurements) in the permeate. The results showed that the membrane with pores` average diameter of 1.36 mu m achieved higher transmembrane flux than the membrane with pores` average diameter of 0.8 mu m. The volume of open pores (responsible for the permeation) was predominant in the total porosity, which was higher than 50% for all tested membranes. Concerning demulsification, the monolayer membranes were efficacious, as the rejection coefficient was higher than 99%.

Silicon carbide surface modification by nitrogen plasma expander

Silicon carbide (SiC) has been employed in many different fields such as ballistic armor, thermal coating, high performance mirror substrate, semiconductors devices, among other things. Plasma application over the silicon carbide ceramics is relatively recent and it is able to promote relevant superficial modifications. Plasma expander was used in this work which was supplied by nitrogen and switched by a capacitor bank. Nitrogen plasma was applied over ceramic samples for 20 minutes, in a total medium of 1440 plasma pulses. SiC ceramics were produced by uniaxial pressing method (40 MPa) associated to isostatic pressing (300 MPa) and sintered at 1950 degrees C under argon gas atmosphere. Silicon carbide (beta-sic - BF-12) supplied by HC-Starck and sintering additive (7.6% YAG - Yttrium Aluminum Garnet) were used in order to obtain the ceramics. Before and after the plasma application, the samples were characterized by SEM, AFM, contact angle and surface energy measurement.

Production of a low young modulus titanium alloy by powder metallurgy

Titanium alloys have several advantages over ferrous and non-ferrous metallic materials, such as high strengthto-weight ratio and excellent corrosion resistance. A blended elemental titanium powder metallurgy process has been developed to offer low cost commercial products. The process employs hydride-dehydride (HDH) powders as raw material. In this work, results of the Ti-35Nb alloy sintering are presented. This alloy due to its lower modulus of elasticity and high biocompatibility is a promising candidate for aerospace and medical use. Samples were produced by mixing of initial metallic powders followed by uniaxial and cold isostatic pressing with subsequent densification by isochronal sintering between 900 up to 1600 °C, in vacuum. Sintering behavior was studied by means of microscopy and density. Sintered samples were characterized for phase composition, microstructure and microhardness by X-ray diffraction, scanning electron microscopy and Vickers indentation, respectively. Samples sintered at high temperatures display a fine plate-like alpha structure and intergranular beta. A few remaining pores are still found and density above 90% for specimens sintered in temperatures over 1500 °C is reached.

Obtenção in situ do compósito alfa-SiAlON-SiC

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Sintering of tin oxide using zinc oxide as a densification aid

The physicochemical electronic characteristics of SnO2 render it useful in many technical applications, including ceramic varistors, stable electrodes used in electric glass-melting furnaces and electrometallurgy of aluminum, transparent windows and chemical sensors. The use of ZnO as a sintering aid was explored in this study to obtain SnO2 as a dense ceramic. Compacts were obtained by mechanical mixing of oxides, isostatic pressing at 210 MPa and sintering in situ inside a dilatometer at heating rates of 10degreesC/min. The grain size and microstructure were investigated by scanning and transmission electron microscopy (SEM/TEM). The phases and chemical composition were analyzed by energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The results indicated that ZnO acts as a densification aid for SnO2, improving its grain growth with additions of up to 2 mol%. ZnO forms a solid solution with SnO2 UP to 1 mol%, above which SnZnO3 precipitates in the grain boundary, potentially inhibiting shrinkage and grain growth. (C) 2004 Kluwer Academic Publishers

Development of alpha-SiAlON-SiC ceramic composites by liquid phase sintering

In this work, in situ alpha-SiAlON-SiC ceramic composites were obtained,by, liquid phase sintering, using SiC as reinforcement. Different beta-SiC powder contents (0-20 wt.%), were added to Si3N4-AlN-RE2O3. powder mixtures, and compacted by cold isostatic pressing. The samples were sintered at 1950 degrees C for 1 h, in N-2 atmosphere. Sintered: samples were characterized by relative density, weight loss, X-ray diffraction and scanning electron microscopy. Furthermore, mechanical properties such as hardness and fracture toughness were determined by Vickers indentation method. Lattice parameters of the alpha' phase did not considerably change with increase of SiC content. However, morphology, average grain size and aspect ratio of the alpha' phase were considerably changed with increase of the SiC content. These behavior influences significantly the mechanical properties of this hard ceramic composite. (C) 2006 Elsevier Ltd. All rights reserved.

Isochronal sintering of the blended elemental Ti-35Nb alloy

Titanium alloy parts are ideally suited for advanced aerospace systems and surgical implants because of their unique combination of high specific strength at both room temperature and moderately elevated temperature, in addition to excellent corrosion resistance. In this work, results of the Ti-35Nb alloy sintering are presented. This alloy, due to its lower modulus of elasticity and high biocompatibility, is a promising candidate for surgical and aerospace applications. Samples were produced by mixing of initial metallic hydride powders followed by uniaxial and cold isostatic pressing with subsequent densification by isochronal sintering between 700 and 1500 degrees C, in vacuum. Sintering behavior was studied by means of microscopy and density. Sintered samples were characterized for phase composition, microstructure and microbardness by X-ray diffraction, scanning electron microscopy and Vickers indentation, respectively. Samples sintered at high temperatures display a fine plate-like a structure and intergranular P. A few remaining pores are still found, and density above 97% for specimens sintered at 1500 degrees C is reached. (c) 2007 Elsevier B.V. All rights reserved.

Production of Ti-35Nb alloy by powder metallurgy for aerospace application

Titanium and its alloys provide high strength-to-weight ratios, good fatigue strength and increased corrosion resistance compared with others materials. Its acceptance in aerospace has been limited by costs considerations such as high cost of raw material, high buy-to-fly ratios and expensive machining operations. Significant cost reductions can be obtained by vacuum sintering and powder metallurgy (P/M) techniques by producing near net shapes and consequently minimizing material waste and machining time. The Ti 35Nb alloy exhibit a low modulus of elasticity. Stemming from the unique combination of high strength, low modulus of elasticity and low density, this alloy is intrinsically more resistant to shock and explosion damages than most other engineering materials. Samples were produced by mixing of initial metallic powders followed by uniaxial and cold isostatic pressing with subsequent densification by sintering between 900 and 1600 °C, in vacuum. Sintering behavior was studied by means of dilatometry. Sintered samples were characterized for phase composition, microstructure and microhardness by X-ray diffraction, scanning electron microscopy and Vickers indentation, respectively. Density was measured by Archimedes method. Copyright © 2004 Society of Automotive Engineers, Inc.

Development of silicon carbide substrates for aerospace applications

Payload and high-tech are important characteristics when the goals are aerospace applications. The development of the technologies associated to these applications has interests that transcend national boundaries and are of strategic importance to the nations. Ultra lightweight mirrors, supports and structures for optical systems are important part of this subject. This paper reports the development of SiC substrates, obtained by pressing, to be applied on embedded precision reflective optics. Different SiC granulometries, having YAG as sintering additive, were processed by: ball milling, drying and deagglomeration, sift, uniaxial and isostatic pressing, and, finally, argon atmosphere sintering at 1900°C. Different porosities were obtained according to the amount of organic material added. Into one side of the samples pellets of organic material were introduced to generate voids to reduce the weight of samples as a whole. The substrates were grinding and polished, looking for a SiC surface having low porosity, as porosity is directly related to light scattering that should be avoided on optical surfaces. Laser surface treatments were applied (using or not SiC barbotine) as a method to improve the surface quality. The samples were characterized by optical and laser confocal microscopy, roughness measurements and mechanical tests. The results are very promissory for future applications. © 2012 Materials Research Society.