Papers by Keyword: Transmission Electron Microscopy (TEM)

Abstract: This work deals with the microstructural evolution of creep resistant martensitic/ferritic 11% Cr-steel during thermomechanical treatment from an experimental as well as modeling point of view. The creep resistance of this material group is highly dependent on the precipitate status. The initial precipitate status is controlled by the chemical composition of the alloy and the heat treatment after casting or hot rolling. It is therefore of utmost interest to understand and model the precipitate kinetics during this process. Once the microstructural evolution has been modeled successfully, only minimum effort is required to computationally test variants in the composition or heat treatment in order to optimize the process. In this work, the material was hot rolled, austenitized and subsequently annealed. All heat treatments have been performed during dilatometry tests. In order to investigate the microstructural evolution during the process, specimens were extracted at definite stages of the treatment. The specimens were then investigated applying various microscopical techniques in order to quantify the microstructural features (grain size, martensite lath width and precipitate data). The experimental data were then compared to thermodynamic simulations (MatCalc). General data such as nucleation sites for precipitates were taken from literature, grain size and martensite lath widths from the experimental data. Simulations include equilibrium calculations and precipitate kinetic simulations. In general, the simulations showed good agreement with the experimental findings, with minor room for improvements. The work thus lays a solid ground for future improvements of the heat treatment process.

Abstract: Texture evolution in two magnesium alloys, Mg-4%Zn-1%Nd and Mg-1%Zn-1%Nd (weight percentage), was studied after rolling and the subsequent isothermal annealing. The finish rolling was completed in a single pass with a thickness reduction rate of ~30% at 100 °C and a rolling speed of 1000 m/min. After cooling to room temperature, the rolled samples were annealed at 350 °C for different annealing times. Upon annealing, the maximum intensity of the basal pole texture decreases as recrystallization progresses. In the Mg-1Zn-1Nd alloy (with a high Nd/Zn ratio), texture weakening is maintained even after complete recrystallization and grain coarsening, while in the Mg-4Zn-1Nd alloy, texture strengthening occurs after grain coarsening, and a single peak replaces the double split basal peaks. In the Mg-1Zn-1Nd alloy, grain coarsening is accompanied by a bimodal grain size distribution, whereas in the Mg-4Zn-1Nd alloy, the grain coarsening leads to a uniform grain size distribution. TEM investigations show the formation of the Zn and Nd rich clusters at early stage of annealing in both alloys. During recrystallization, these clusters were dissolved in the Mg-4Zn-1Nd alloy, but they are more stable in the Mg-1Zn-1Nd alloy. In our opinion, the formation of these stable clusters is one of the main factors for texture weakening of the Mg-Zn-RE alloys.

Abstract: In the framework of the made researches nanocomposite of CNT-NPs type (Carbon Nanotube-Nanoparticles) consisting of multiwalled carbon nanotubes coated by rhodium nanoparticles and/or palladium using the two-step indirect method: chemical reduction have been produced. In the researches high-quality multi-walled carbon nanotubes MWCNTs with a length of 100 to 500 nm and a diameter of 8 to 20 nm previously obtained in the catalytic-chemical vapour deposition CCVD have been used. Nanotubes produced within the framework of own researches contain minor amounts of metallic impurities and amorphous carbon deposits. In order to deposit the noble metal nanoparticles on the surface of carbon nanotubes functionalization of multi-walled carbon nanotubes in a mixture of H₂SO₄ and HNO₃ acids have been used. The prepared material has been subjected chemical reduction using noble metal precursors (RhCI₃, PdCl₂). The characterization of the produced material including the examination of the structure, morphology, chemical composition and evaluation of the size and distribution of rhodium and/or palladium nanoparticles on the surface of carbon nanotubes has been performed using: scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS). The produced nanomaterials may be used as the active layer of sensors of chemical/biological agents.

Abstract: Hydride precipitation due to the spontaneous and fast hydrogen diffusion is often pointed as causing embrittlement and rupture in zirconium alloys used in the nuclear industry. Transmission Electron Microscopy (TEM) and X-Rays Diffraction (XRD) have been used to study the precipitation of hydride phases in zirconium alloys as a function of the hydrogen content. The orientation relationships observed between the hydride phase and the substrate were similar to those previously observed in Titanium hydrides grown on Titanium. Dislocation emission from the hydride precipitates has been directly related to the relaxation of the misfit stresses appearing during the transformation. The stability of the hydride phases after several dissolution-reprecipitation cycles have been studied by DSC, TEM and XRD for different total hydrogen content in several alloys. The energy of precipitation observed is lower than that of the dissolution in each case studied. The temperature associated with these two processes slightly increase as a function of the cycle number, as a result of the homogenizing hydrogen distribution in the alloy bulk. The same hydrides phases present before cycling were also observed after 20 cycles. However, transition phases poorer in hydrogen than the dominant one may precipitate at the interface with the substrate. The evolution of these transitions phases with the temperature increase will be investigated by TEM in-situ heating in the next future.

Abstract: Nanostructured W₇₀Cr₃₀ powders were produced by mechanical alloying (MA) of elemental tungsten (W), Chromium (Cr) powders in a high energy planetary ball-mill using tungsten carbide as grinding media and toluene as a process control agent. The crystallite size and lattice strain of the nanostructured powders at different milling time (0 h to 10 h) was calculated from X-ray diffraction patterns (XRD). The crystallite size of W in W₇₀Cr₃₀ powder reduced from 100 μm at 0 h to 32.8 nm at 10 h of milling with increase in lattice strain of 0.43% at 10 h of milling. The lattice parameter of tungsten shows initial expansion of lattice upto 0.56% at 5 h of milling and contraction of lattice upto 0.93% at 10 h of milling. The scanning electron microscopy (SEM) micrograph also revealed mixed morphology of elemental W and Cr powders consist of spherical and elongated particles during mechanical alloying (0 h to 10 h). The dark-field transmission electron microscopy (TEM) observations indicated that the crystallite size (~30 nm) of W in W-Cr alloy in the as-milled powder is in good agreement with calculated crystallite size from XRD. Maximum solid solubility of 4.4 at.% Cr in W was found at 10 h of milling. The dislocation density increases from 6.75 (10¹⁶/m²) to 17.56 (10¹⁶/m²) with increase in the milling time from 0 h to 20 h. No cracks in the sintered pellets were visible under scanning electron microscope (SEM). Hardness and Elastic Modulus of sintered W₇₀Cr₃₀ alloy determined by nanoindentation test are less compared to pure W.

Abstract: The plasmodynamic synthesis was conducted in the electric hypervelocity pulse jet of carbon-silicon electric discharge plasma influenced on a copper target in an argon atmosphere. Some samples of a powder product with a high content of β-SiC were produced. The results of the experiments made at different levels of supplied energy were compared. It was shown that the sizes of crystals grew, when the energy of a plasma shot increased.

Abstract: Polyacrylamide (PAM) was chemically anchored to the surface of multi-walled carbon nanotubes (MWCNTs) by atom transfer radical polymerization (ATRP) of acrylamide (AM). It started from the functional groups such as –COOH on the sidewall of MWCNTs, which derived from the oxidation of carbon nanotubes. FT-IR and ¹H NMR results shown that the multi-walled carbon nanotubes grafted PAM (MWCNT-g-PAM) have been successfully carried out. The MWCNT-g-PAM showed different relative weight loss kinetics with PAM determined by thermal gravimetric analysis (TGA). The transmission electron microscopy (TEM) shown that the PAM grafted polymer was wrapped on the surface of carbon nanotubes.

Abstract: We report a facile hydrothermal synthesis in base solution for shape/size-controlled ceria (CeO₂) nanocrystals and CeO₂-ZrO₂ solid solution. CeO₂ nanocrystals in the shape of nanorods, nanotubes, or nanocubes with reactive {110} and {200} faces can be produced using this hydrothermal method. We found that hydrothermal reaction temperature is a critical parameter to control the shape and size of ceria nanocrystals. Above 210 °C, high resolution transmission electron microscopy studies revealed that the CeO₂ nanocubes expose predominant {200} crystal planes. Microscopic investigation showed that the CeO₂-ZrO₂ solid solutions synthesized using this method had high crystallinity, and compositional homogeneity, and improved low-temperature reducibility.

Abstract: An efficient synthesis route is proposed to obtain single powder CaFe₅O₇ ceramic. This complex structure can be described as an intergrowth between one CaFe₂O₄ unit and n= 3 slices of FeO Wustite-type structures. A fine structural study has been carried out at room temperature by transmission electron microscopy (TEM) observations (ED and HREM). The analysis of these data has revealed a supercell with a monoclinic symmetry associated to some twinning phenomena. From the hkl conditions deduced to electron diffraction study, the centrosymmetric P2₁/m setting can be proposed. This monoclinic cell exhibit close relationships with the previous one reported as orthorhombic (a_o =3.05 Å, b_o = 10.05 Å and c_o = 18 Å) according to the following metric a_m=2c_o, b_m=c_o, c_m=b_o/2sinβ and β=106.74°.

Abstract: The effect on hardness and precipitate microstructure of elastically straining a 6060 Al-Mg-Si alloy during natural ageing or artificial ageing has been investigated. The elastic strain is here defined as 50 % of the material yield strength. All heat treatments where elastic straining was applied led to an increased hardness compared to the unstrained reference material. Quantitative investigations of the precipitate microstructure using transmission electron microscopy (TEM) did not indicate any significant difference in precipitate parameters as compared to the unstrained reference material. Therefore the increased strength in the elastically strained material is being linked to strain induced dislocations based on faster ageing kinetics compared to unstrained reference samples.