Synergistic effects of anisotropy and image force on TEM diffraction contrast of dislocation loops.

Based on column approximation (CA) assumption, many-beam Schaeublin-Stadelmann diffraction equations are employed for simulating the transmission electron microscopy (TEM) diffraction image contrast of dislocation loops within thin TEM foil of finite thickness, and two beam and many beam diffraction conditions are compared. Moreover, the effects of materials anisotropy and free surface relaxation induced elastic fields distortion of dislocation loops on the black-white image contrast are specially focused. It is found that anisotropy has a remarkable impact on the TEM image contrast of dislocation loop, and free surface relaxation induced image forces can change the black-white contrast features when dislocation loops are near TEM foil free surfaces. Thus, in order to make reliable judgment on the nature of defects, effects of free surface and anisotropy should be included when analysing irradiation induced dislocation loops and other type of defects in in-situ electron, proton, heavy-ion irradiation experiments under TEM environments.

The role of zinc in the biocorrosion behavior of resorbable Mg‒Zn‒Ca alloys.

Zinc- and calcium-containing magnesium alloys, denominated ZX alloys, excel as temporary implant materials because of their composition made of physiologically essential minerals and lack of commonly used rare-earth alloying elements. This study documents the specific role of nanometric intermetallic particles (IMPs) on the in vitro and in vivo biocorrosion behavior of two ZX-lean alloys, Mg‒Zn1.0‒Ca0.3 (ZX10) and Mg‒Zn1.5‒Ca0.25 (ZX20) (in wt.%). These alloys were designed according to thermodynamic considerations by finely adjusting the nominal Zn content towards microstructures that differ solely in the type of phase composing the IMPs: ZX10, with 1.0 wt.% Zn, hosts binary Mg2Ca-phase IMPs, while ZX20, with 1.5 wt.% Zn, hosts ternary IM1-phase IMPs. Electrochemical methods and the hydrogen-gas evolution method were deployed and complemented by transmission electron microscopy analyses. These techniques used in concert reveal that the Mg2Ca-type IMPs anodically dissolve preferentially and completely, while the IM1-type IMPs act as nano-cathodes, facilitating a faster dissolution of ZX20 compared to ZX10. Additionally, a dynamically increasing cathodic reactivity with progressing dissolution was observed for both alloys. This effect is explained by redeposits of Zn on the corroding surface, which act as additional nano-cathodes and facilitate enhanced cathodic reaction kinetics. The higher degradation rate of ZX20 was verified in vivo via micro-computed tomography upon implantation of both materials into femurs of Sprague DawleyⓇ rats. Both alloys were well integrated with direct bone‒implant contact observable 4 weeks post operationem, and an appropriately slow and homogeneous degradation could be observed with no adverse effects on the surrounding tissue. The results suggest that both alloys qualify as new temporary implant materials, and that a minor adjustment of the Zn content may function as a lever for tuning the degradation rate towards desired applications. STATEMENT OF SIGNIFICANCE: In Mg‒Zn‒Ca (ZX)-lean alloys Zn is the most electropositive element, and thus requires special attention in the investigation of biocorrosion mechanisms acting on these alloys. Even a small increase of only 0.5 wt.% Zn is shown to accelerate the biodegradation rate in both simulated body conditions and in vivo. This is possible due to Zn's role in influencing the type of intermetallic particles (IMPs) in these alloys. These IMPs in turn, even though minute in size, are shown to govern the biocorrosion behavior on the macroscopic scale. The deep understanding gained in this study on the role of Zn and of the IMP type it governs is crucial to ensuring a safe and controllable implant degradation.

Three-dimensional scanning transmission electron microscopy of dislocation loops in tungsten.

Scanning transmission electron microscopy (STEM) imaging using diffraction contrast is a powerful technique to assess crystal defects. In this work it is used to assess the spatial distribution of radiation induced defect in tungsten. In effect, its irradiation leads to the formation of nanometric dislocation loops that under certain conditions may form intriguing 3-D rafts. In this study, we have irradiated thin tungsten samples in situ in a TEM with 1.2 MeV W ions to 0.017 dpa at room temperature (RT) and at 700 °C. Besides the Burgers vector analysis, the number density and size of the dislocation loops with their spatial arrangement were quantitatively characterized by stereo imaging in STEM mode. Most of the loops have a Burgers vector ½ a0 〈111〉, with some a0 〈100〉 at room temperature. Loops are located mainly in the simulated damage profile but there is also a significant portion in deeper regions of the sample, indicating that loops in W diffuse easily, even at RT. At 700 °C, loops form elongated rafts that contain dislocation segments having a Burgers vector ½ a0 〈111〉. The rafts are narrow and reside on {111} planes; they are elongated along 〈110〉 directions, which correspond, when combined to the rafts' Burgers vector, to the lines of edge dislocations. Compared to conventional TEM, 3-D analysis in STEM appears thus as a powerful technique for quantitative analyses of defects in tungsten, as it allows reducing the background diffraction contrast and reaching thicker areas of the electron transparent foil, here 0.5 µm of tungsten at 200 kV.

Monotropic polymorphism in a glass-forming metallic alloy.

This study investigates the crystallization and phase transition behavior of the amorphous metallic alloy Au70Cu5.5Ag7.5Si17. This alloy has been recently shown to exhibit a transition of a metastable to a more stable crystalline state, occurring via metastable melting under strong non-equilibrium conditions. Such behavior had so far not been observed in other metallic alloys. In this investigation fast differential scanning calorimetry (FDSC) is used to explore crystallization and the solid-liquid-solid transition upon linear heating and during isothermal annealing, as a function of the conditions under which the metastable phase is formed. It is shown that the occurrence of the solid-liquid-solid transformation in FDSC depends on the initial conditions; this is explained by a history-dependent nucleation of the stable crystalline phase. The microstructure was investigated by scanning and transmission electron microscopy and x-ray diffraction. Chemical mapping was performed by energy dispersive x-ray spectrometry. The relationship between the microstructure and the phase transitions observed in FSDC is discussed with respect to the possible kinetic paths of the solid-liquid-solid transition, which is a typical phenomenon in monotropic polymorphism.

Weak beam under convergent beam illumination

The weak beam technique is now used widely for the determination of stacking fault energies, in particular for intermetallic alloys, and the accuracy of the approach is critically dependent upon the reliability of the relationship between the image and the actual position of the dissociated dislocations. Examining as a model case a dislocation dissociated into two Shockley partial dislocations in Cu at 100 kV for orientations ranging through the g(3g) weak beam condition, image simulations are used to explore the accuracy to which the true spacing between the partial dislocations can be determined from the spacing measured on the image as a function of the dislocation character, the foil thickness, the dislocation depth in the foil, the diffraction condition and the beam convergence. It appears that for image simulations and for the given conditions a beam convergence of about 5 mrad allows to greatly improve the accuracy, and that beam convergence must be taken into account quantitatively when deducing the true partial dislocation spacing as it is the principal parameter controlling the precision in this type of measurement.

Structure analysis by diffraction of amorphous zones created by Ni ion implantation into pure Al

The implantation of Ni ions into pure Al leads to the formation of approximately 10 nm amorphous zones (AZ) which induce diffuse rings in the diffraction pattern in addition to the diffraction spots of the crystal. Measurements by energy dispersive spectrometry and electron energy loss spectrometry attributed to the amorphous zones an average Ni concentration of 25 at%. The exact structure of these AZ is still unknown. The structure is characterized here by both the total and partial radial distribution functions (RDF). Structure factor deduced from experiments is compared to calculated one. For this purpose, molecular dynamic (MD) simulations are used to model the AZ structure. The RDF are determined using this structure and analytical calculation of the diffraction pattern is achieved. Simulations of the diffraction pattern of the simulated MD sample using both a kinematic and a dynamic approach are achieved to refine the analytical procedure used on the experimental diffraction patterns. It appears that the amorphous structure is well reproduced by the MD simulations. Analytical calculation reveals the presence of a well-established chemical order in the amorphous material.