scholarly journals Implementation of the Chicot–Lesage Composite Hardness Model in a Determination of Absolute Hardness of Copper Coatings Obtained by the Electrodeposition Processes

Metals ◽  
2021 ◽  
Vol 11 (11) ◽  
pp. 1807
Author(s):  
Ivana O. Mladenović ◽  
Jelena S. Lamovec ◽  
Dana G. Vasiljević-Radović ◽  
Rastko Vasilić ◽  
Vesna J. Radojević ◽  
...  
Keyword(s):  
Preferred Orientation ◽  
Sulfate Electrolyte ◽  
X Ray Diffraction ◽  
Fine Grained ◽  
Atomic Force ◽  
Copper Coatings ◽  
Hardness Model ◽  
Composite Hardness ◽  
Coating Hardness

The influence of various electrolysis parameters, such as the type of cathode, composition of the electrolyte and electrolysis time, on the morphology, structure and hardness of copper coatings has been investigated. Morphology and structure of the coatings were analyzed by scanning electron microscope (SEM), atomic force microscope (AFM) and X-ray diffraction (XRD), while coating hardness was examined by Vickers microindentation test applying the Chicot–Lesage (C–L) composite hardness model. Depending on the conditions of electrolysis, two types of Cu coatings were obtained: fine-grained mat coatings with a strong (220) preferred orientation from the sulfate electrolyte and smooth mirror bright coatings with a strong (200) preferred orientation from the electrolyte with added leveling/brightening additives. The mat coatings showed larger both measured composite and calculated coating hardness than the mirror bright coatings, that can be explained by the phenomena on boundary among grains. Independent of electrolysis conditions, the critical relative indentation depth (RID) of 0.14 was established for all types of the Cu coatings, separating the zone in which the composite hardness can be equaled with the coating hardness and the zone requiring an application of the C–L model for a determination of the absolute hardness of the Cu coatings.

scholarly journals Determination of the absolute hardness of electrolytically produced copper coatings by application of the Chicot-Lesage composite hardness model

2021 ◽  
pp. 105-105
Author(s):  
Ivana Mladenovic ◽  
Jelena Lamovec ◽  
Dana Vasiljevic-Radovic ◽  
Vesna Radojevic ◽  
Nebojsa Nikolic
Keyword(s):  
Pause Duration ◽  
Atomic Force ◽  
Copper Coatings ◽  
The Absolute ◽  
Hardness Model ◽  
Composite Hardness ◽  
Pulsating Current ◽  
Good Agreement ◽  
Coating Hardness

In this study, a novel procedure based on application of the Chicot?Lesage (C?L) composite hardness model was proposed for determination of an absolute hardness of electrolytically produced copper coatings. The Cu coatings were electrodeposited on the Si(111) substrate by the pulsating current (PC) regime with a variation of the following parameters: the pause duration, the current density amplitude and the coating thickness. The topography of produced coatings was characterized by atomic force microscope (AFM), while a hardness of the coatings was examined by Vickers microindentation test. Applying the C?L model, the critical relative indentation depth (RID)c of 0.14 was determined, which is independent of all examined parameters of the PC regime. This RID value separated the area in which the composite hardness of the Cu coating corresponded to its absolute hardness (RID < 0.14) from the area in which application of the C?L model was necessary for a determination of the absolute coating hardness (RID ? 0.14). The obtained value was in a good agreement with the value already published in the literature.

scholarly journals Application of the Composite Hardness Models in the Analysis of Mechanical Characteristics of Electrolytically Deposited Copper Coatings: The Effect of the Type of Substrate

Metals ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 111
Author(s):  
Ivana O. Mladenović ◽  
Nebojša D. Nikolić ◽  
Jelena S. Lamovec ◽  
Dana Vasiljević-Radović ◽  
Vesna Radojević
Keyword(s):  
Mechanical Characteristics ◽  
Dislocation Creep ◽  
Average Current Density ◽  
Fine Grained ◽  
Copper Coatings ◽  
Electrochemically Deposited ◽  
Composite Models ◽  
Average Current ◽  
Composite Hardness ◽  
Coating Hardness

The mechanical characteristics of electrochemically deposited copper coatings have been examined by application of two hardness composite models: the Chicot-Lesage (C-L) and the Cheng-Gao (C-G) models. The 10, 20, 40 and 60 µm thick fine-grained Cu coatings were electrodeposited on the brass by the regime of pulsating current (PC) at an average current density of 50 mA cm−2, and were characterized by scanning electron (SEM), atomic force (AFM) and optical (OM) microscopes. By application of the C-L model we determined a limiting relative indentation depth (RID) value that separates the area of the coating hardness from that with a strong effect of the substrate on the measured composite hardness. The coating hardness values in the 0.9418–1.1399 GPa range, obtained by the C-G model, confirmed the assumption that the Cu coatings on the brass belongs to the “soft film on hard substrate” composite hardness system. The obtained stress exponents in the 4.35–7.69 range at an applied load of 0.49 N indicated that the dominant creep mechanism is the dislocation creep and the dislocation climb. The obtained mechanical characteristics were compared with those recently obtained on the Si(111) substrate, and the effects of substrate characteristics such as hardness and roughness on the mechanical characteristics of the electrodeposited Cu coatings were discussed and explained.

scholarly journals Photocatalytic Bi2O3/TiO2:N Thin Films with Enhanced Surface Area and Visible Light Activity

Coatings ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 445
Author(s):  
Luís P. Dias ◽  
Filipe C. Correia ◽  
Joana M. Ribeiro ◽  
Carlos J. Tavares
Keyword(s):  
Visible Light ◽  
Surface Area ◽  
Selective Absorption ◽  
X Ray Diffraction ◽  
Force Microscopy ◽  
Β Phase ◽  
Atomic Force ◽  
Light Activity ◽  
Vls Growth

Bi2O3 nanocone films functionalized with an overlayer of TiO2 were deposited by d.c. reactive magnetron sputtering. The aforementioned nanocone structures were formed via a vapour-liquid-solid (VLS) growth, starting from a catalytic bismuth seed layer. The resultant nanocones exhibit an improved surface area, measured by atomic force microscopy, when compared to non-VLS deposition of the same metal oxide. X-ray diffraction texture analysis enabled the determination of the crystallographic β-phase of Bi2O3. A very thin TiO2 overlayer (6 nm thick), undoped and doped with nitrogen, was deposited onto the nanocones template, in order to functionalize these structures with a photocatalytic, self-cleaning, cap material. N-doped TiO2 overlayers increased the selective absorption of visible light due to nitrogen doping in the anatase cell, thus, resulting in a concomitant increase in the overall photocatalytic efficiency.

Determination of the Residual Stress Field around Scratches Using Synchrotron X-Rays and Nanoindentation

2010 ◽  
Vol 652 ◽  
pp. 25-30
Author(s):  
M.K. Khan ◽  
Michael E. Fitzpatrick ◽  
L.E. Edwards ◽  
S.V. Hainsworth
Keyword(s):  
Residual Stress ◽  
Stress Field ◽  
Residual Stresses ◽  
Small Scale ◽  
X Rays ◽  
X Ray Diffraction ◽  
Residual Stress Field ◽  
Fine Grained ◽  
Load Displacement

The residual strain field around the scratches of 125µm depth and 5µm root radius have been measured from the Synchrotron X-ray diffraction. Scratches were produced using different tools in fine-grained aluminium alloy AA 5091. Residual stresses up to +1700 micro-strains were measured at the scratch tip for one tool but remained up to only +1000 micro-strains for the other tool scratch. The load-displacement curves obtained from nanoindentation were used to determine the residual stresses around the scratches. It was found that the load-displacement curves are sensitive to any local residual stress field present and behave according to the type of residual stresses. This combination of nanoindentation and synchrotron X-rays has been proved highly effective for the study of small-scale residual stresses around the features such as scratches.

scholarly journals Quantitative Determination of Preferred Orientation by Energy-Dispersive X-Ray Diffraction

1976 ◽  
Vol 2 (2) ◽  
pp. 95-111 ◽  
Author(s):  
L. Gerward ◽  
S. Lehn ◽  
G. Christiansen
Keyword(s):  
Quantitative Determination ◽  
Rolling Texture ◽  
Tension Test ◽  
Preferred Orientation ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fibre Texture

The use of energy-dispersive X-ray diffraction for quantitative determination of preferred orientations in polycrystalline specimens is analysed. The method is applied to determinations of rolling texture and fibre texture. The adaptability of the method to in situ studies is demonstrated by observations of texture changes simultaneous with the deformation of a specimen in a tension test.

scholarly journals Characterizing the microstructural anisotropy of fine-grained phyllosilicate-rich rocks

2021 ◽  
Vol 1 ◽  
pp. 69-70
Author(s):  
Rebecca Kühn ◽  
Michael Stipp ◽  
Bernd Leiss
Keyword(s):  
Physical Properties ◽  
Texture Analysis ◽  
High Energy ◽  
Preferred Orientation ◽  
Low Grade ◽  
X Ray Diffraction ◽  
Crystallographic Preferred Orientation ◽  
X Ray ◽  
Fine Grained ◽  
Microstructural Anisotropy

Abstract. The physical properties of claystones, shales, and slates are highly dependent on the alignment of phyllosilicate minerals. With increasing overburdening, the shape and the crystallographic preferred orientation of these minerals are affected by uniaxial shortening as well as tectonic processes including recrystallization under elevated pressure and temperature conditions. The microstructural anisotropy expressed mainly by the alignment of phyllosilicates significantly predetermines the orientation of fractures, hence the shear strength and stability of clay-rich sediments and rocks. A quantitative analysis of phyllosilicate alignment is therefore essential to evaluate the properties and the mechanical behavior of these rocks. This can be carried out by analyzing the crystallographic preferred orientation (texture). Although texture analysis is a common tool in geosciences, it becomes more difficult in fine-grained rocks owing to for example particle size, heterogeneity, the polyphase composition, and difficulties in sample preparation. Methods such as electron backscatter diffraction, neutron diffraction, or laboratory X-ray diffraction are restricted with respect to preparation artifacts, sampling size and statistics, water content, etc. To overcome these issues, we successfully apply high-energy X-ray diffraction as available at synchrotron research facilities, e.g., at the German Electron Synchrotron Facility (DESY) in Hamburg, Germany, or the European Synchrotron Research Facility (ESRF) in Grenoble, France. In combination with Rietveld refinement we analyze the bulk texture of phyllosilicate-rich rocks. Here we present the results of texture analysis from a wide range of these rocks: Pleistocene poorly consolidated mud (rocks), affected only by sedimentation and burial; more highly consolidated but tectonically largely unaffected Jurassic claystone from the Opalinus Formation of the Swabian Alb; Carboniferous shales from the Harz mountains representing low-grade metamorphic and deformed rocks. Our methodical approach to quantifying the microstructural anisotropy using texture analysis in fine-grained rocks allows for the quantification of physical properties resulting from the alignment of phyllosilicates. Furthermore, it enables the prediction of direction-dependent mechanical strength, which is crucial for the establishment of long-term repositories for radioactive waste in shales and claystones.

X-Ray Diffraction Determination of Texture and Stress in Damascene Fabricated Copper Interconnects

1999 ◽  
Vol 563 ◽  
Author(s):  
Delrose Winter ◽  
Paul R. Besser
Keyword(s):  
Incident Beam ◽  
Preferred Orientation ◽  
Copper Interconnects ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Determination ◽  
Lattice Planes ◽  
Excellent Tool

AbstractX-Ray diffraction (XRD) provides an excellent tool for the measurement of both stress and texture (preferred orientation) on fabricated damascene interconnect structures. Since x-ray diffraction provides a direct measurement of lattice spacings, film strain can be measured directly. Also, since the intensity of diffracted x-rays is proportional to the density of lattice planes oriented in diffracting condition with respect to the incident beam, both the direction and extent of preferred orientation can be accurately measured. Special techniques and considerations are necessary when examining damascene interconnect structures with XRD which are not necessary with blanket films. These techniques are discussed and described in order to aid in obtaining meaningful XRD data and a correct interpretation of the results.

Epitaxial Growth of Copper Film by MOCVD

2016 ◽  
Vol 680 ◽  
pp. 507-510 ◽  
Author(s):  
Rong Tu ◽  
Jin Huang ◽  
Song Zhang ◽  
Lian Meng Zhang
Keyword(s):  
Epitaxial Growth ◽  
Copper Film ◽  
Preferred Orientation ◽  
Copper Films ◽  
X Ray Diffraction ◽  
Atomic Force ◽  
Metal Organic ◽  
Single Crystal Sapphire ◽  
Substrate Temperatures ◽  
Electronic Microscope

Copper thin films were deposited on single crystal sapphire substrate via metal-organic MOCVD using Cu (acac)2 as precursor. X-ray diffraction (XRD) and Scanning Electronic Microscope (SEM) were employed for studying preferred orientation and microstructure. Atomic Force Microscope was utilized in order to characterize roughness of copper thin layer. By calculation of the Gibbs free energy, the reactions have been deeply understood. Depositions were carried out at various substrate temperatures in the rage 473K to 673K. It has been revealed that temperature determined the orientation and microstructure of copper films. At 673K, copper films have exhibited preferred orientation, smooth surface and connected grains, which proved that this copper thin film can act as precursor. Based on the study of epitaxial growth of copper films, a schematic diagram of epitaxial growth relationship is suggested for the step by step depositions processes.

Stress-Depth Profiles in Magnetron Sputtered Mo Films Using Grazing Incidence X-Ray Diffraction (GIXD)

1993 ◽  
Vol 37 ◽  
pp. 189-196 ◽  
Author(s):  
B. L. Ballard ◽  
P. K. Predecki ◽  
D. N. Braski
Keyword(s):  
Grazing Incidence ◽  
X Ray Diffraction ◽  
Vycor Glass ◽  
X Ray ◽  
Force Microscopy ◽  
Fine Grained ◽  
Atomic Force ◽  
Grazing Incidence Diffraction ◽  
Composition Profiles ◽  
Deposition Mode

AbstractIntrinsic stresses as a function of σ, the 1/e penetration depth were measured for a smooth, 1μm thick, fine grained, cylindrical post magnetron sputtered molybdenum film deposited on a vycor glass substrate in the dynamic deposition mode. Using grazing incidence diffraction and the Mo (321) reflection, lattice spacing profiles were determined for τ values from 200-4400 Å. The in-plane intrinsic stresses parallel and perpendicular to the post axis were determined employing the ϕ-integral method and assuming elastic isotropy. The results were related to the surface structure and composition profiles via atomic force microscopy (AFM) and auger electron spectroscopy (AES) respectively.

scholarly journals Morphology, Structure and Mechanical Properties of Copper Coatings Electrodeposited by Pulsating Current (PC) Regime on Si(111)

Metals ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 488 ◽  
Author(s):  
Ivana O. Mladenović ◽  
Jelena S. Lamovec ◽  
Dana G. Vasiljević Radović ◽  
Rastko Vasilić ◽  
Vesna J. Radojević ◽  
...  
Keyword(s):  
Current Density ◽  
Diffusion Control ◽  
Copper Electrodeposition ◽  
Average Current Density ◽  
Fine Grained ◽  
Average Current ◽  
Hardness Model ◽  
Xrd Techniques ◽  
Composite Hardness ◽  
Pulsating Current

Copper electrodeposition on (111)-oriented Si substrate was performed by the pulsating current (PC) regime at various average current densities in the range of 15–70 mA·cm−2, obtained by varying either the frequency (30, 50, 80 and 100 Hz for the current density amplitude of 100 mA·cm−2) or the current density amplitude (120 and 140 mA·cm−2 at 100 Hz). The produced Cu coatings were examined by SEM, AFM and XRD techniques. The morphology of the coatings changed from those with large grains to fine-grained and globular, while the crystal structure changed from the strong (220) to the strong (111) preferred orientation by increasing the average current density. The mechanical characteristics of coatings were examined using Vickers micro-indentation tests, applying the Chicot–Lesage (C–L) composite hardness model for the analysis of microhardness. The maximum microhardness was obtained for the Cu coating produced at an average current density of 50 mA·cm−2, with a current density amplitude of 100 mA·cm−2 and a frequency of 100 Hz. This copper coating was fine-grained and showed the smallest roughness in relation to the other coatings, and it was obtained in the mixed activation–diffusion control between the end of the effect of the activation control and the beginning of the dominant effect of diffusion control.

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