In-Situ Tem Investigation During Thermal Cycling of thin Copper Films

1996 ◽  
Vol 436 ◽  
Author(s):  
R.-M. Keller ◽  
W. Sigle ◽  
S. P. Baker ◽  
O. Kraft ◽  
E. Arzt

AbstractIn-situ transmission electron microscopy (TEM) was performed to study grain growth and dislocation motion during temperature cycles of Cu films with and without a cap layer. In addition, the substrate curvature method was employed to determine the corresponding stresstemperature curves from room temperature up to 600°C. The results of the in-situ TEM investigations provide insight into the microstructural evolution which occurs during the stress measurements. Grain growth occurred continuously throughout the first heating cycle in both cases. The evolution of dislocation structure observed in TEM supports an explanation of the stress evolution in both capped and uncapped films in terms of dislocation effects.

1988 ◽  
Vol 100 ◽  
Author(s):  
M. W. Bench ◽  
I. M. Robertson ◽  
M. A. Kirk

ABSTRACTTransmission electron microscopy experiments have been performed to investigate the lattice damage created by heavy-ion bombardments in GaAs. These experiments have been performed in situ by using the HVEN - Ion Accelerator Facility at Argonne National Laboratory. The ion bcorbardments (50 keV Ar+ and Kr+) and the microscopy have been carried out at temperatures rangrin from 30 to 300 K. Ion fluences ranged from 2 × 1011 to 5 × 1013 ions cm−2.Direct-inpact amorphization is observed to occur in both n-type and semi-insulating GaAs irradiated to low ion doses at 30 K and room temperature. The probability of forming a visible defect is higher for low temperature irradiations than for room temperature irradiations. The amorphous zones formed at low temperature are stable to temperatures above 250 K. Post implantation annealing is seen to occur at room temperature for all samples irradiated to low doses until eventually all visible damage disappears.


1994 ◽  
Vol 364 ◽  
Author(s):  
A. Korner

AbstractThe domain structure and the evolution of antiphase boundaries (APBs) have been investigated in Fe-Al by means of “in-situ” transmission electron microscopy (TEM) heating experiments. Single crystals with composition Fe22.1at%Al and Fe25.6at%Al have been used.The grown-in structure of the Fe22.1at%al single crystal is composed of DO3 ordered particles embedded in the disorderd ±-matrix. A bimodal distribution of the particles was found. Small ordered particles are in between the large precipitates which are surrounded by particle-free zones. Numerous of this large ordered precipitates contain APBs. Crossing the transition temperature to the disordered phase, the small particles dissolve into the ±-matrix and the large particles start to shrink by dissolving.The single crystal with composition Fe25.6at%Al was found to be completely DO3 ordered. The grown-in domains are separated by APBs of type a′0/2〈100〉. At temperatures far below the transition temperature to the B2 phase no significant change in the APB and domain structure has been detected. In contrast, a remarkable evolution in the APB structure has been observed approaching the transition temperature. Coarsening of the domains has been found. Furthermore, APBs of B2-type (a′0/4〈lll〉 shear) are dragged out by dislocation motion. B2- and DC3-type APBs react and junctions are formed. With increasing annealing time, the density of B2-type boundaries increases. The TEM image is dominated by B2-type boundaries linked by the D03-type boundaries. The DO3 superlattice spots are clearly excited approaching the transition temperature to B2. Above the transition temperature, the DO3 spots disappear completely and the diffraction pattern reveals B2 long range order.


1995 ◽  
Vol 404 ◽  
Author(s):  
John S. Vetrano ◽  
Steve M. Bruemmer ◽  
Ian M. Robertson

AbstractRecrystallization and grain growth studies of Al-Mg-Mn-Zr alloys have been carried out in-situ in the transmission electron microscope. Nucleation sites were primarily on large (>I μm diameter) eutectic constituent particles. The sub-micron A16Mn dispersoids were observed to be effective as nuclei if present in clusters, and were effective at retarding grain boundary migration and dislocation motion. The smaller A13Zr precipitates seemed to have little effect on nucleation and growth, but were effective in pinning dislocations. These results have been analyzed in terms of precipitate size and shape in both the as-cold-worked microstructure and during recrystallization. The implications on the microstructural refinement of these alloys for improved superplastic properties will be discussed.


2006 ◽  
Vol 976 ◽  
Author(s):  
Bryan Miller ◽  
Jamey Fenske ◽  
Dong Su ◽  
Chung-Ming Li ◽  
Lisa Dougherty ◽  
...  

AbstractDeformation experiments at temperatures between 300 and 750 K have been performed in situ in the transmission electron microscope to investigate dislocation interactions and reactions with grain boundaries and other obstacles. Dislocations, both partial and perfect, as well as deformation twins have been observed being emitted from grain boundaries and, in some cases, even the same grain boundary. The ejection of dislocations from the grain boundary can result in its partial or total annihilation. In the latter case, the disintegration of the grain boundary was accompanied by grain growth and a change in misorientation.


1994 ◽  
Vol 343 ◽  
Author(s):  
Munir D. Naeem ◽  
Stephen M. Rossnagel ◽  
Krishna Rajan

ABSTRACTWe have studied the effects of low energy ion bombardment on thin copper films. Evaporated, sputtered and CVD copper films (∼50 nm) were exposed to Magnetically Enhanced (ME) Ar plasmas. The microstructural changes (grain size) in the films were studied using Transmission Electron Microscopy (TEM).Grain growth is observed in thin Cu films when the films are exposed to low energy (87 eV) Ar plasmas. The microstructural changes in sputtered and evaporated films are quite significant whereas the plasma bombardment has less effect on CVD films. These changes occur very rapidly and cannot be attributed solely to the thermal effects, especially at low RF power levels (500 W). The initial microstructure of the film has a significant effect on grain growth during plasma exposure.


2004 ◽  
Vol 854 ◽  
Author(s):  
K. Hattar ◽  
J. Gregg ◽  
J. Han ◽  
T. Saif ◽  
I. M. Robertson

ABSTRACTIn situ transmission electron microscopy analysis is used to study the stability of nanograined and ultra-fine grained thin films at elevated temperatures. In the free-standing Au and Cu films, grain growth was dependent on annealing temperature and time with growth observed in both materials at temperatures greater than 373K. Both materials exhibited abnormal grain growth although it was more prevalent in Au than in Cu, which may be a consequence of pinning of the Cu grain boundaries by impurities. The formation and destruction of twins was observed to play a critical role in the grain growth, with the twins retarding the growth in gold, but not in Cu. In constrained Au films no grain growth was observed on annealing at temperatures below 636 K. At 636 K, the eutectic temperature, the microstructure transformed to the eutectic structure with the first stage being the annihilation of the grain structure.


2017 ◽  
Vol 197 ◽  
pp. 337-351 ◽  
Author(s):  
G. Marien Bremmer ◽  
Eirini Zacharaki ◽  
Anja O. Sjåstad ◽  
Violeta Navarro ◽  
Joost W. M. Frenken ◽  
...  

Using a MEMS nanoreactor in combination with a specially designed in situ Transmission Electron Microscope (TEM) holder and gas supply system, we imaged the formation of multiple layers of graphene encapsulating a cobalt nanoparticle, at 1 bar CO : N2 (1 : 1) and 500 °C. The cobalt nanoparticle was imaged live in a TEM during the Boudouard reaction. The in situ/operando TEM studies give insight into the behaviour of the catalyst at the nanometer-scale, under industrially relevant conditions. When switching from Fischer–Tropsch syngas conditions (CO : H2 : N2 1 : 2 : 3 at 1 bar) to CO-rich conditions (CO : N2 1 : 1 at 1 bar), we observed the formation of multi-layered graphene on Co nanoparticles at 500 °C. Due to the high temperature, the surface of the Co nanoparticles facilitated the Boudouard reaction, causing CO dissociation and the formation of layers of graphene. After the formation of the first patches of graphene at the surface of the nanoparticle, more and more layers grew over the course of about 40 minutes. In its final state, around 10 layers of carbon capped the nanoparticle. During this process, the carbon shell caused mechanical stress in the nanoparticle, inducing permanent deformation.


Author(s):  
Vasily Bulatov ◽  
Wei Cai

In the preceding chapters we have discussed several computational approaches focused on the structure and motion of single dislocations. Here we turn our attention to collective motion of many dislocations, which is what the method of dislocation dynamics (DD) was designed for. Typical length and time scales of DD simulations are on the order of microns and seconds, similar to in situ transmission electron microscopy (TEM) experiments where dislocations are observed to move in real time. In a way, DD simulations can be regarded as a computational counterpart of in situ TEM experiments. One very valuable aspect of such a “computational experiment” is that one has full control of the simulation conditions and access to the positions of all dislocation lines at any instant of time. Provided the dislocation model is realistic, DD simulations can offer important insights that help answer the fundamental questions in crystal plasticity, such as the origin of the complex dislocation patterns that emerge during plastic deformation and the relationship between microstructure, loading conditions and the mechanical strength of the crystal. So far, two approaches to dislocation dynamics simulations have emerged. In the line DD method to be discussed in this chapter, dislocations are represented as mathematical lines in an otherwise featureless host medium. An alternative approach is to rely on a continuous field of eigenstrains, in which regions of high strain gradients reveal the locations of the dislocation lines. This representation leads to the phase field DD approach, which will be discussed in Chapter 11. Line DD has certain similarities with the models discussed in the previous chapters, but, at the same time, is rather different from all of them. For example, the representation of dislocations by line segments in line DD method is similar to the kinetic Monte Carlo (kMC) model of Chapter 9. However, having to deal with multiple dislocations on large length and times scales necessitates a more economical treatment of dislocations in the line DD method. Thus, line DD usually relies on less detailed discretization of dislocation lines and treats dislocation motion as deterministic.


2005 ◽  
Vol 907 ◽  
Author(s):  
David M. Follstaedt ◽  
Khalid Hattar ◽  
James A. Knapp ◽  
Ian M. Robertson

AbstractIn situ transmission electron microscopy was used to show that nanocrystalline nickel produced by pulsed-laser deposition undergoes abnormal grain growth at moderate temperatures (225-400°C). The growth rate was found to increase with thickness for the three film thicknesses examined, 50, 80 and 150 nm. The abnormal growth proceeded in an irregular manner: initiation sites and growth direction were unpredictable, and the grains exhibited no preferred orientation. Some abnormal grains show internal boundaries such as twins, while others exhibited lattice misalignments across the grain body. The grains contain many defects, including dislocations, stacking faults and surprisingly, stacking fault tetrahedra. The stacking fault tetrahedra are not a result of quenching nor of electron irradiation-induced lattice displacements; they instead are thought to form from vacancies trapped in the growing grain as it incorporates lower-density material at the high-angle grain boundaries in the nanocrystalline matrix.


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