Thermally induced hillock formation in Al–Cu films

1989 ◽  
Vol 4 (5) ◽  
pp. 1172-1181 ◽  
Author(s):  
C. Y. Chang ◽  
R. W. Vook

Isothermal annealing studies of hillocks formed on Al–15 wt.% Cu films, vapor deposited at 25 °C on oxidized silicon wafers, were carried out in situ in a scanning electron microscope. The original hillocks formed as a result of substrate-induced thermal expansion strains which caused material to diffuse out of the film to form the hillocks when the films were heated to the isothermal annealing temperatures. During isothermal annealing the hillock density decreased and the average size of the hillocks increased. Measurements of these quantities as a function of time were made at a series of temperatures ranging from 200 to 300 °C. The activation energies for these two cases were found to be 0.29 and 0.28 eV, respectively. X-ray energy spectroscopy analysis of the films showed that the hillocks were richer in copper than the matrix. Transmission electron microscopy showed that the average hillock and grain sizes in the variously annealed films were linearly related and of the same order of magnitude. The results were also analyzed using Chakraverty's models for surface and interfacial diffusion. It was concluded that the evidence clearly shows that the observed processes could be well characterized by a typical Ostwald ripening model.

Author(s):  
Mihaela Albu ◽  
Bernd Panzirsch ◽  
Hartmuth Schröttner ◽  
Stefan Mitsche ◽  
Klaus Reichmann ◽  
...  

Powder and SLM additively manufactured parts of X5CrNiCuNb17-4 maraging steel were systematically investigated by electron microscopy to understand the relationship between the properties of the powder grains and the microstructure of the printed parts. We prove that satellites, irregularities and superficial oxidation of powder particles can be transformed into an advantage through the formation of nanoscale (AlMnSiTiCr)-oxides in the matrix during the printing process. The nano-oxides showed extensive stability in terms of size, spherical morphology, chemical composition and crystallographic disorder upon in situ heating up to 950°C in the scanning transmission electron microscope. Their presence thus indicates a potential for oxide-dispersive strengthening of this steel, which may be beneficial for creep resistance at elevated temperatures. The nucleation of copper clusters and their evolution into nanoparticles as well as the precipitation of Ni and Cr particles upon in situ heating have as well been systematically documented.


2000 ◽  
Author(s):  
D. L. Tu ◽  
A. Kar ◽  
X. L. Wu

Abstract Titanium carbide particle (TiCp)-reinforced Ni alloy composite coatings are synthesized by laser cladding using a cw 3 kW CO2 laser. Two kinds of coatings are possible in terms of the origin of TiCp: undissolved TiCp and in-situ generated TiCp. The former originates from the TiCp pre-coated on the sample whereas the latter from in-situ chemical reaction between titanium and graphite in the molten pool during laser irradiation. For the coating reinforced by TiCp formed in-situ, the sub-micron TiCp particles are formed and uniformly distributed because of the in-situ reaction and trapping effect during rapid solidification. Graded distribution of TiCp is obtained on a macro scale. The volume fraction increases from 1.86% at the coating-substrate interface to 38.4% at the coating surface. For the coating reinforced by undissolved TiCp, analytical transmission electron microscopy (ATEM) and high resolution transmission electron microscopy (HRTEM) observations show the existence of the epitaxial growth of TiC, the precipitation of CrB and M23C6, and the chemical reaction between Ti and B elements around phase interfaces of undissolved TiCp. In the matrix near the phase interface of undissolved TiCp, the loading curve obtained by nanoindenter exhibits pop-in phenomena due to the plastic deformation of cracks or debonding of TiCp from the matrix. For TiCp generated in-situ, no pop-in mark appears, indicating high fracture toughness. Coating with TiCp generated in-situ exhibits higher hardness and modulus than the coating with undissolved TiCp at regions near the phase interface. The coating reinforced by TiCp generated in-situ also displays higher impact wear resistance and abrasive wear resistance compared to the coatings with undissolved TiCp and without TiCp respectively.


2022 ◽  
Author(s):  
Xinchuang Zhang ◽  
Mei Wu ◽  
Bin Hou ◽  
Xuerui Niu ◽  
Hao Lu ◽  
...  

Abstract In this work, the N2O radicals in-situ treatment on gate region has been employed to improve device performance of recessed-gate AlGaN/GaN high-electron-mobility transistors (HEMTs). The samples after gate recess etching were treated by N2O radicals without physical bombardment. After in-situ treatment (IST) processing, the gate leakage currents decreased by more than one order of magnitude compared to the sample without IST. The fabricated HEMTs with the IST process show a low reverse gate current of 10-9 A/mm, high on/off current ratio of 108, and high fT×Lg of 13.44 GHz·μm. A transmission electron microscope (TEM) imaging illustrates an oxide layer with a thickness of 1.8 nm exists at the AlGaN surface. X-ray photoelectron spectroscopy (XPS) measurement shows that the content of the Al-O and Ga-O bonds elevated after IST, indicating that the Al-N and Ga-N bonds on the AlGaN surface were broken and meanwhile the Al-O and Ga-O bonds formed. The oxide formed by a chemical reaction between radicals and the surface of the AlGaN barrier layer is responsible for improved device characteristics.


1977 ◽  
Vol 99 (4) ◽  
pp. 634-640
Author(s):  
T. W. Thompson ◽  
S. Sen ◽  
K. E. Gray ◽  
T. F. Edgar

Tests have been carried out to quantify the variation in permeability of Texas lignite with drying and with applied stress. It has been shown that the matrix permeability of lignite may be increased from effectively zero to the order of 10 darcies by removing about 20 percent by weight of water. In addition, an increase of confining pressure after drying will reduce the permeability, but only by about one order of magnitude. Drying of the matrix thus may produce matrix permeabilities of the same order as the undried field fracture permeability. The permeability increase of the matrix is initially greater parallel to the bedding than perpendicular, but after further drying the two orientations show similar final permeabilities. This drying effect could have a significant influence on the operation of an in-situ gasification process by increasing the transmissivity and injectivity of the producing seam. Drying of the seam could occur by the flow of unsaturated gas and will be enhanced by combustion.


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.


Materials ◽  
2019 ◽  
Vol 12 (1) ◽  
pp. 172 ◽  
Author(s):  
Ming Li ◽  
Zhiming Shi ◽  
Xiufeng Wu ◽  
Huhe Wang ◽  
Yubao Liu

In this work, the microstructure of Al-5Fe-1.5Er alloy was characterized and analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS) techniques. The effect of microstructure on the behavior of crack initiation and propagation was investigated using in situ tensile testing. The results showed that when 1.5 wt.% Er was added in the Al-5Fe alloy, the microstructure consisted of α-Al matrix, Al3Fe, Al4Er, and Al3Fe + Al4Er eutectic phases. The twin structure of Al3Fe phase was observed, and the twin plane was {001}. Moreover, a continuous concave and convex interface structure of Al4Er was observed. Furthermore, Al3Fe was in the form of a sheet with a clear gap inside. In situ tensile tests of the alloy at room temperature showed that the crack initiation mainly occurred in the Al3Fe phase, and that the crack propagation modes included intergranular and trans-granular expansions. The crack trans-granular expansion was due to the strong binding between Al4Er phases and surrounding organization, whereas the continuous concave and convex interface structure of Al4Er provided a significant meshing effect on the matrix and the eutectic structure.


2020 ◽  
Vol 321 ◽  
pp. 11035
Author(s):  
E. Sukedai ◽  
E. Aeby-Gautier ◽  
M. Dehmas

A Ti-5553 specimen was continuously heated to 923 K and simultaneously in-situ HEXRD profiles were taken. In addition, specimens heated at the same rate to several temperatures up to 923 K and further quenched were observed by transmission electron microscopy. Based on both results obtained, transformation sequence was clarified, precipitations of ω-, α”iso- and α-phases were confirmed, and size and density of these precipitates were measured. Hardness values of those specimens were also measured. The hardening mechanism was considered as shearing-mechanism for specimens aged at lower temperatures and by-pass one for specimens aged at higher temperature. An attempt of distinction between α”iso - and α-precipitates was also tried. Both precipitates were in needle-like shape and a possibility was suggested by measuring angles between two needle-shape precipitates on {110} of the matrix and comparing with each other.


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.


1988 ◽  
Vol 134 ◽  
Author(s):  
C. Robin Hwang ◽  
Michael F. Malone ◽  
Richard J. Farris ◽  
David C. Martin ◽  
Edwin L. Thomas

ABSTRACTA novel method of preparing PBZT/nylon composite fibers by infiltrating nylon into pure PBZT fiber is described. The pure PBZT fiber formed a microfibrillar network structure during coagulation, which is effective in reinforcing the matrix in the “in-situ network” composite fibers (designated IC). These new composite fibers exhibit nearly indistinguishable mechanical properties as those of “molecular” composite fibers (MC) prepared from isotropic solutions before and after tension heat-treatment (E = 44 GPa, σ = 430 MPa, ε = 1.2 %, σc = 250 MPa, G = 1.75 GPa) for PBZT/nylon weight ratios equal to unity.The fine structure of pure PBZT and its composite fibers spun from isotropic solutions was characterized using techniques based on nitrogen adsorption, small-angle X-ray scattering, scanning and transmission electron microscopies. The structure of both type of composites was found to be a microfibrillar network of PBZT in a matrix of amorphous nylon. The average diameters of the PBZT microfibrils were in the range of 10 to 20 nm for the IC and 4 nm for the MC.


2017 ◽  
Vol 263 ◽  
pp. 50-54
Author(s):  
Waraporn Piyawit ◽  
Panya Buahombura

CuAgZr alloy is a minor variation of CuAg alloy that is remarkably known for good combination of strength and electrical conductivity. Strengthening and conductivity enhancing of CuAgZr alloy is essentially proficient by the precipitation of Ag precipitates. The behavior of Ag precipitates at high temperature was investigated using in-situ transmission electron microscopy. These nanoscale Ag precipitates are formed in CuAgZr alloy during heating process with the average size of 5 nm. Growth of precipitates at higher temperature can be explained by the consumption of solute diffusing from smaller precipitates. Dislocation looping at high temperature would be the effects of a large lattice strain along matrix/precipitate interface that would retard the dislocation movement.


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