Papers by Keyword: TEM Analysis

Abstract: Specimens from Ni-Cr-Fe wrought superalloy INCONEL 718 were used for fatigue push-pull test at elevated temperature 700 °C. Fatigue loading was with the coefficient of cycle asymmetry R = -1. Temperature of fatigue test was chosen from two reasons; one is that limit operating temperature for this type of alloy is 650 – 700 °C due to precipitation of stable but incoherent orthorhombic Ni₃Nb delta phase; the second reason for this temperature is fact that metastable body-centred tetragonal Ni₃Nb gamma double prime phase starts to transform to delta phase and from that reason there is an expectation for mechanical properties decreasing due to increased volume of delta phase. For evaluation of fatigued specimens were Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) observation used. Also methods of quantitative metallography – coherent testing grids were used for evaluation of delta phase volume. Some references describe that higher volume of delta phase, mostly situated at grain boundaries, act as initiation sites for cracks and therefore decreasing mechanical properties. Employed SEM and TEM analysis confirm the increased volume of delta phase in specimens after fatigue loading but a negative influence on dynamic properties, such fatigue lifetime, for this alloy was not confirmed.

Abstract: Thermo-mechanical treatment, in particular, cryo-rolling is a unique technique to produce super high strength AA-7xxx aluminium alloys with ultra-fine grained structure. In order to conduct the rolling at room temperature and cryo-temperature (liquid N₂ (-190°C)), the AA-7xxx alloy ingot was rolled from 6mm to 1mm with 85% reduction in thickness. Optical microscopy, XRD, electron microscopy, hardness and tensile testing were conducted on the rolled alloy for understanding the phase changes and evaluating the mechanical properties. The alloy rolled at liquid nitrogen (LN₂) exhibits very high strength with reasonable ductility. Corrosion behaviour of AA-7xxx series aluminium alloy various conditions in NaCl (3.5%) solution were investigated. Cold rolled and cryo rolled alloy exhibits better corrosion resistance than that of cast.

Abstract: Metallographic analyses on microstructure of squeeze cast magnesium alloy AM50 with different levels of calcium addition are performed via optical microscopy (OM), and scanning electron microscopy (SEM). The OM results show the calcium has a grain refining effect on the base alloy AM50 with the level of Ca addition up to 2 wt.%. As the Ca content further increases, its grain refining effect becomes limited. The SEM observation reveals the addition of 2 wt.% Ca to the AM50 alloy leads to the formation of a continuous network of eutectic phases along grain boundaries while the discontinuous divorced secondary eutectic β-Mg₁₂Al₁₇ is present in the microstructure of AM50 containing also the primary α-Mg, and Mn-Al intermetallic particles. The elemental mapping by the energy dispersive spectroscopy (EDS) indicates the presence of the major alloying elements of Al and Ca along grain boundaries in the squeeze cast AM50 alloy with Ca addition.

Abstract: One challenge for volume manufacturing of 4H-SiC devices is the state-of-the-art wafer dicing technology – the mechanical blade dicing which suffers from high tool wear and low feed rates. In this paper we discuss Thermal Laser Separation (TLS) as a novel dicing technology for large scale production of SiC devices. We compare the latest TLS experimental data resulting from fully processed 4H-SiC wafers with results obtained by mechanical dicing technology. Especially typical product relevant features like process control monitoring (PCM) structures and backside metallization, quality of diced SiC-devices as well as productivity are considered. It could be shown that with feed rates up to two orders of magnitude higher than state-of-the-art, no tool wear and high quality of diced chips, TLS has a very promising potential to fulfill the demands of volume manufacturing of 4H-SiC devices.

Abstract: Mechanical blade dicing is a state-of-the-art technique for the chip separation of SiC devices. Due to the hardness of SiC this technique suffers from low feed rate and high wear of the diamond coated dicing blade, resulting in the risk of uncontrolled tool breakage during the dicing process. With the upcoming transition to 150 mm diameter of SiC wafers this technique will most probably reach its limit. For dicing SiC wafers of those diameters on a productive scale three alternative dicing technologies are considered in this paper: ablation laser dicing, Stealth Dicing and Thermal Laser Separation. All these methods are based on laser processing. The benefits of these technologies are discussed in detail and compared to the classical mechanical diamond blade dicing, including a brief summary of first experimental results on each of the three laser dicing technologies.

Abstract: Commercial nanopowder of the partially yttrium-stabilized zirconia (ZrO₂+3 mol.% Y₂O₃) was treated by the non-cavitational powerful ultrasonic action (PUA). Influence of PUA on the microstructure and phase composition of the powder has been investigated by scanning and transmission electron microscopy. Investigated powder before and after PUA has polycrystalline structure. It was found that TZ-3YS particles after PU-treatment have tetragonal and cubic zirconia phases; some of the particles consist of a mixture of monoclinic, tetragonal and cubic phases, but these particles have substructure with random orientation of fragments.

Abstract: 3C-SiC/Si heteroepitaxy is hampered by large mismatches in lattice parameters (19.7%) and thermal expansion coefficient (8%) leading to 3C-SiC films containing high defects density. To reduce the presence of defects, a multi-step growth process in a CVD reactor is used. The aim of the work is to study the effect of carbonization on differently oriented Si surfaces, experiencing a 200°C-wide temperature range in a CVD reactor, to improve the crystalline quality. TEM analysis are carried out to evaluate thickness, crystal orientations and defects of carbonized layers with respect to the time-dependence of the process and to the different orientations of the Si substrate. It will be shown that process-related defects are strictly correlated to the substrate orientation either for size, density, occupied area, shape or thickness. Uniform, flat and crystalline thin SiC films are obtained with a low defect density.

Abstract: Titanium oxynitride (TiOxNy) films were prepared by RF PECVD on Si(100) and glass substrates using nitrogen and argon mixture gas. Titanium iso-propoxide (Ti[OCH(CH3) 2] 4, 97%) was used as precursor with different nitrogen flow rate to control oxygen and nitrogen contents in the films. Changes of chemical states of constituent elements in the deposited films were examined by X-ray photoelectron spectroscopy (XPS) analysis. With increasing nitrogen flow rate the total amount of nitrogen was increased while that of oxygen was decreased. The film growth orientation and N-H peak intensity characteristics were also analyzed by X-ray diffraction (XRD), atomic force microscopy (AFM), and infrared spectroscopy (FT-IR). Through refractive index as well as contact angle analysis, we can suggest that relationship to surface energy and optical property. Moreover, transmission electron microscopy (TEM) was also used to investigate the morphology of TiOxNy thin film and the phase of the TiOxNy thin film different nitrogen flow rate.

Abstract: Hollow polystyrene nanocapsules with sizes of ~100 nm have been prepared via a miniemulsion polymerization process by applying the encapsulation of a nonsolvent (i.e., isooctane). Divinylbenzene has been added to styrene as a cross-linking comonomer in order to improve a structural stability of the hollow polymer capsules. Morphology variation of nanocapsules with concentrations of divinylbenzene and also isooctane has been studied using transmission electron microscopy analysis. Kinetic study on the miniemulsion polymerization of styrene in the presence of divinylbenzene and isooctane has been carried out using fractional conversion data determined by the gravimetric analysis.

Abstract: Excellent mechanical properties (high strength and toughness) of microalloyed steels are mainly caused by induced precipitation during thermomechanical treatment (TMT) and grain refinement. It has been recently found that TMT of Nb-microalloyed steels can give rise to two different kinds of precipitates, manifested by the double plateau in the statically recrystallised fraction (Xa) against time curves. This work presents an electron diffraction study performed in a transmission electron microscope, equipped with an EDS analytical system. Lattice parameters of a great deal of particles, smaller than 200 nm and with face cubic centred structure, have been measured. Frequency distribution of the values of lattice parameters shows that these are grouped in two sets whose mean values are close. Comparison of these values with those found in the literature for carbides, nitrides and carbonitrides usually present in microalloyed steels demonstrates that they are Nb carbonitrides with slight stoichiometric differences (NbCxNy).