This in situ transmission electron microscopy work presents a nanoscale characterization of the microstructural evolution in 3D-printed Inconel 718 (IN718) while exposed to elevated temperature and an associated change in the mechanical property under tensile loading. Here, we utilized a specially designed specimen shape that enables tensile testing of nano-sized thin films without off-plane deformations. Additionally, it allows a seamless transition from the in situ heating to tensile experiment using the same specimen, which enables a direct correlation of the microstructure and the mechanical property of the sample. The method was successfully used to observe the residual stress relaxation and the formation of incoherent γ′ precipitates when temperature was increased to 700°C. The subsequent in situ tensile test revealed that the exposure of the as-printed IN718 to a high temperature without full heat treatment (solutionizing and double aging) leads to loss of ductility.

Sintering of a palladium catalyst supported on alumina (Al2O3) in an oxidizing environment was studied by in situ transmission electron microscopy (TEM). In the case of a fresh catalyst, sintering of Pd particles on an alumina surface in a 500 mTorr steam environment happened via traditional ripening or migration and coalescence mechanisms and was not significant unless heating above 500°C. After the catalyst was used for the hydrogenation of alkynes, TEM coupled with convergent beam electron diffraction and electron energy loss spectroscopy analysis revealed that most of the Pd particles were lifted from the alumina surface by hydrocarbon buildup. This dramatically different morphology totally changed the sintering mechanism of Pd particles during the regeneration process. Catalytic gasification of hydrocarbon around these particles in an oxidizing environment allowed the Pd particles to move around and coalesce with each other at temperatures as low as 350°C. For catalysts heating under 500 mTorr steam at 350°C, steam stripped hydrocarbon catalytically at the beginning, but the reaction stopped after 4 h. Heating in air resulted in both catalytic and noncatalytic stripping of hydrocarbon.

The reactions which occur between amorphous carbon and a number of first transition metals (Ti, Cr, Fe, Co, Ni, and Cu) have been studied by transmission electron microscopy (TEM). The materials are in thin-film form with the metal layer sandwiched between thicker carbon layers. In four cases, the predominant reaction is the graphitization of the amorphous carbon, at temperatures well below 800°C. This is brought about by the elements themselves in the case of Co and Ni, and by metastable carbides in the case of Fe (Fe3C) and Cr (Cr3C2−x). The Ti–C and Cu–C systems do not exhibit graphitization. For the former, only TiC is produced up to 1000°C, while the carbon does not react at all with copper. In situ TEM studies show the mechanism to be of the dissolution-precipitation type, which is equivalent to the metal-mediated crystallization process for amorphous silicon and germanium. The heat of graphitization is found to be 18–19 kcal/mol-C by differential scanning calorimetry.

Reduction of Cr(VI) by the bacterium, Shewanella oneidensis (previously classified Shewanella putrefaciens strain MR-1), was studied by absorption spectrophotometry and in situ, environmental cell–transmission electron microscopy (EC-TEM) coupled with electron energy loss spectroscopy (EELS). Bacteria from rinsed cultures were placed directly in the environmental cell of the transmission electron microscope and examined under 100 Torr pressure. Bright field EC-TEM images show two distinct populations of S. oneidensis in incubated cultures containing Cr(VI)O42−: those that exhibit low image contrast and heavily precipitateencrusted cells exhibiting high image contrast. Several EELS techniques were applied to determine the oxidation state of Cr associated with encrusted cells. The encrusted cells are shown to contain a reduced form of Cr in oxidation state +3 or lower. These results demonstrate the capability to determine the chemistry and valence state of reduction products associated with unfixed, hydrated bacteria in an environmental cell transmission electron microscope.

Nanomaterials have attracted a great deal of research interest recently. The small size of nanostructures constrains the applications of well-established testing and measurement techniques, thus new methods and approaches must be developed for quantitative measurement of the properties of individual nanostructures. This article reports our progress in using in situ transmission electron microscopy to measure the electrical, mechanical, and field-emission properties of individual carbon nanotubes whose microstructure is well-characterized. The bending modulus of a single carbon nanotube has been measured by an electric field-induced resonance effect. A nanobalance technique is demonstrated that can be applied to measure the mass of a tiny particle as light as 22 fg (1 fg = 10−15 g), the smallest balance in the world. Quantum conductance was observed in defect-free nanotubes, which led to the transport of a superhigh current density at room temperature without heat dissipation. Finally, the field-emission properties of a single carbon nanotube are observed, and the field-induced structural damage is reported.

In this work, the high-temperature behavior of nanocrystalline TiO2 is studied using in situ transmission electron microscopy (TEM). These nanoparticles are made using wet chemical techniques that generate the anatase phase of TiO2 with average grain sizes of 6 nm. X-ray diffraction studies of nanophase TiO2 indicate the material undergoes a solid-solid phase transformation to the stable rutile phase between 600° and 900°C. This phase transition is not observed in the TEM samples, which remain anatase up to temperatures as high as 1000°C. Above 1000°C, nanoparticles become mobile on the amorphous carbon grid and by 1300°C, all anatase diffraction is lost and larger (50 nm) single crystals of a new phase are present. This new phase is identified as TiC both from high-resolution electron microscopy after heat treatment and electron diffraction collected during in situ heating experiments. Video images of the particle motion in situ show the nanoparticles diffusing and interacting with the underlying grid material as the reaction from TiO2 to TiC proceeds.

We describe here real-time, in situ observations of the formation of nanosize germanium (Ge) islands on silicon (Si). The deposition of Ge onto electron-transparent Si(100) takes place in a UHV transmission electron microscope that has been modified to allow chemical vapor deposition to be carried out in the polepiece. We recorded the growth process at video rate and were therefore able to follow the evolution of individual islands. As the islands grew, we observed a coarsening process similar to classical Ostwald ripening, but which leads at certain times to a bimodal distribution of island sizes. We show that this phenomenon can be understood using a model in which a conventional coarsening process is modified by a transition between two different island shapes.

Strained layer heterostructures provide ideal systems with which to study the dynamics of dislocation motion via in situ transmission electron microscopy, as the geometry, strain state, and kinetics can be characterized and directly controlled. We discuss how these structures are used to study dislocation-point defect interactions, emphasizing the experimental requirements necessary for quantification of dislocation motion. Following ion implantation, different concentrations and types of point defects are introduced within the SiGe epilayer depending on the implantation species, energy, and current density. By annealing samples in situ in the transmission electron microscope (TEM) following implantation, we can directly observe dislocation motion and quantify the effect of dislocation-point defect interactions on dislocation velocities. We find that dislocation motion is impeded if the implantation dose peak lies within the epilayer, as dislocations pin at point defect atmospheres. Shallow BF2 implantation into the sample capping layer results in more complicated behavior. For low current density implants, dislocation velocities may be dramatically increased; at higher current densities the magnitude of this increase is significantly smaller. Implantation of different ions separately implicates fluorine as the species responsible for the observed increases in dislocation velocities, presumably due to an electrical effect on the rate of dislocation kink nucleation.