Anodic Oxidation of Titanium in Mixture of β-Glycerophosphate (β-GP) and Calcium Acetate (CA)

2013 ◽  
Vol 594-595 ◽  
pp. 275-280 ◽  
Author(s):  
Hasan Zuhudi Abdullah ◽  
Pramod Koshy ◽  
Charles Christopher Sorrell
Keyword(s):  
Anodic Oxidation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Disodium Salt ◽  
Calcium Acetate ◽  
X Ray Diffraction ◽  
Weak Organic Acid ◽  
Acid Bath ◽  
Ceramic Films ◽  
Glancing Angle

Anodic oxidation is an electrochemical method for the production of a ceramic film on a metallic substrate. It involves the use of an electrical bias at relatively low currents while the substrate is immersed in a weak organic acid bath. The films produced are usually dense and stable, with variable microstructural features. In the present work, ceramic films of the anatase and rutile polymorphs of TiO2were formed on high-purity Ti foil (50 μm) using mixtures of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) solutions. The experiments were carried out at varying voltages (150-350 V), times (1-10 min), and current density (10 mA.cm-2) at room temperature. The ceramic films were characterised using digital photography, glancing angle X-ray diffraction (GAXRD), and field emission scanning electron microscopy (FESEM). The thicknesses of the films on Ti were measured using focused ion beam (FIB) milling. The colour, microstructures, and thicknesses of the films were seen to be strongly dependent on the applied voltage. At bias <200 V, single-phase anatase was observed to form on Ti, while at higher bias (250 V), rutile formed due to the arcing process.

Effect of Current Density on Anodised Titanium in Mixture of β-Glycerophosphate (β-GP) and Calcium Acetate (CA)

2015 ◽  
Vol 1087 ◽  
pp. 212-217 ◽  
Author(s):  
Hasan Zuhudi Abdullah ◽  
Te Chuan Lee ◽  
Maizlinda Izwana Idris ◽  
Charles Christopher Sorrell
Keyword(s):  
Current Density ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Ceramic Coatings ◽  
Disodium Salt ◽  
Calcium Acetate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ceramic Films ◽  
Glancing Angle

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. In this study, the surface morphology and crystallinity of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (1, 3, 5 and 10 min) and current density (10 and 20 mA.cm-2) at room temperature. Anodised titanium was characterised by using glancing angle X-ray diffraction (GAXRD), field emission scanning electron microscope (FESEM) and focused ion beam (FIB) milling. The result of the experiment show that colour, porosity, crystallinity and thickness of the titanium films depended strongly on the current density. More porous surface and large amount of anatase was produced at higher current density. FIB results indicated that the thickness of oxide layer increased as increasing of current density.

Effect of Electrolyte Concentration on Anodised Titanium in Mixture of β-Glycerophosphate (β-GP) and Calcium Acetate (CA)

2015 ◽  
Vol 1087 ◽  
pp. 116-120 ◽  
Author(s):  
Te Chuan Lee ◽  
Maizlinda Izwana Idris ◽  
Hasan Zuhudi Abdullah ◽  
Charles Christopher Sorrell
Keyword(s):  
Oxide Layer ◽  
Applied Voltage ◽  
Focused Ion Beam ◽  
Electrolyte Concentration ◽  
Ion Beam ◽  
Digital Camera ◽  
Disodium Salt ◽  
Calcium Acetate ◽  
Anode Surface ◽  
Ion Diffusion

Anodic oxidation is a surface modification method which combines electric field driven metal and oxygen ion diffusion for formation of oxide layer on the anode surface. Anodised titanium has been widely use in biomedical applications especially in dental implant. This study aimed to investigate the effect of electrolyte concentration on titanium. Specifically, the titanium foil was anodised in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) with different concentration (0.02 M + 0.2 M and 0.04 M + 0.4 M), anodising time (10 min), applied voltage (150, 200, 250, 300 and 350 V) and current density (10 mA.cm-2) at room temperature. Surface oxide properties of anodised titanium were characterised by using glancing angle X-ray diffraction (GAXRD), field emission scanning electron microscope (FESEM), focused ion beam (FIB) milling and digital camera. With increasing electrolyte concentration, the oxide layer became more porous. The GAXRD results also showed that rutile formed at high applied voltage (≥300 V) when the higher concentration of electrolyte was used.

Oxidation of Alloy-X in Subcritical, Transition, and Supercritical Water

CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram
Keyword(s):  
Supercritical Water ◽  
Photoelectron Spectroscopy ◽  
Focused Ion Beam ◽  
Elevated Temperatures ◽  
Subcritical Water ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nickel Based Superalloy ◽  
Before And After

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

Study of Electrochemical Deposition of Copper and Microstructure Evolution in Fine Lines

1999 ◽  
Vol 562 ◽  
Author(s):  
Stephan Grunow ◽  
Deda Diatezua ◽  
Soon-Cheon Seo ◽  
Timothy Stoner ◽  
Alain E. KaloyerosI
Keyword(s):  
Electrochemical Deposition ◽  
Microstructure Evolution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Process Window ◽  
X Ray Diffraction ◽  
Force Microscopy ◽  
Atomic Force ◽  
Underlying Mechanisms ◽  
Pure Cu

ABSTRACTAs computer chip technologies evolve from aluminum-based metallization schemes to their copper-based counterparts, Electrochemical Deposition (ECD) is emerging as a viable deposition technique for copper (Cu) interconnects. This paper presents the results of a first-pass study to examine the underlying mechanisms that control ECD Cu nucleation, growth kinetics, and post-deposition microstructure evolution (self-annealing), leading to the development and optimization of an ECD Cu process recipe for sub-quarter-micron device generations. The influence of bath composition, current waveform, type and texture of Cu seed layer, and device feature size (scaling effect) on the evolution of film texture, morphology, electrical properties, and fill characteristics was investigated using a manufacturing-worthy ReynoldsTech 8″ wafer plating tool. Resulting films were analyzed by X-ray Diffraction (XRD), four-point resistivity probe, Focused-Ion-Beam Scanning Electron Microscopy (FIB-SEM), and Atomic Force Microscopy (AFM). These investigations identified an optimized process window for the complete fill of aggressive device structures with pure Cu with resistivity ∼ 2.0 μΩ-cm and smooth surface morphology.

Characterization of Second-Phase Inclusion in Silicon Carbide Powders

2015 ◽  
Vol 821-823 ◽  
pp. 100-103
Author(s):  
Ta Ching Hsiao ◽  
Shen Tsao ◽  
Sergey Nagalyuk ◽  
Evgeny Mokhov
Keyword(s):  
Silicon Carbide ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Element Distribution ◽  
Second Phase ◽  
X Ray Diffraction ◽  
Dual Beam ◽  
Metal Doped ◽  
Dopant Element

A specific transition metal is used as a dopant element in silicon carbide powders to create the compensation effect. According to ab-initio simulation, vanadium, chromium, and manganese-induced compensation decrease the lifetime of the acceptor carrier and cause higher resistance when boron is the main impurity. Since the silicon carbide lattice has low solubility, excess metal precipitates on the surface of powders, particularly on the grain boundaries. The compositions of matrix and precipitation in the powders reveal obvious differences between the two areas. The X-ray diffraction (XRD) pattern shows the structure of VSi2, which indicates the existence of a second phase. Dual-beam focused ion beam (DBFIB) is used to further analyze the geography inside the powders. A cross-section view by DBFIB shows a second phase in the grains with a composition similar to that in the grain boundary. Metal-doped silicon carbide powders are used as starting materials to conduct crystal growth with better dopant element distribution.

scholarly journals Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study

2021 ◽  
Vol 28 (2) ◽  
pp. 550-565 ◽  
Author(s):  
David Yang ◽  
Nicholas W. Phillips ◽  
Kay Song ◽  
Ross J. Harder ◽  
Wonsuk Cha ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Imaging Study ◽  
X Ray Diffraction ◽  
Multiple Reflections ◽  
X Ray ◽  
Self Diffusion ◽  
Diffraction Imaging ◽  
Gold Microcrystals

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain; however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ∼280°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.

Morphological and Electrical Properties of Silver Thin Films Sputter Deposited on LTCC Substrates

2008 ◽  
Vol 5 (4) ◽  
pp. 169-173 ◽  
Author(s):  
A. Bittner ◽  
T. Bohnenberger ◽  
R. Engel ◽  
H. Seidel ◽  
U. Schmid
Keyword(s):  
Thin Films ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Plasma Power ◽  
X Ray Diffraction ◽  
Deposition Parameters ◽  
Mean Grain Size ◽  
Agglomeration Effects ◽  
Ag Deposition ◽  
Sputter Deposited

Screen printed noble metal thick films are commonly used as metallization on LTCC (low temperature cofired ceramics) substrates. When, however, geometries with a lateral resolution below 20 μm are needed for the realization of devices, alternative techniques are needed, and they are provided by standard thin film technology. To minimize conduction losses, silver (Ag) is favored due to a low bulk resistivity. To evaluate the potential of Ag as metallization, thin films are sputter deposited on glass and LTCC substrates under varying conditions (i.e., plasma power) with different film thicknesses ranging up to 1.75 μm. The microstructure of the Ag films is analyzed applying techniques such as scanning electron microscopy, focused ion beam, and x-ray diffraction. With the latter approach, a mean grain size of about 33 nm is measured independent of plasma power used for Ag deposition. In contrast, the texture strongly varies with deposition parameters resulting in an enhanced generation of (111) planes at higher plasma powers due to an increased adatom mobility. Furthermore, a higher degree in (111) orientation results in a lower resistivity of the Ag films. When the Ag films are postdeposition annealed at 500°C, the resistivity decreases by a factor of 2 compared with the “as deposited” state due to grain growth. Further, sublimation and agglomeration effects dominate leading to an increase in surface roughness and resistivity above average.

Roughening of Au(111) Surfaces During Ion Beam Erosion: A Scanning Tunneling Microscope and X-Ray Diffraction Study

1999 ◽  
Vol 570 ◽  
Author(s):  
A. Judy ◽  
M.V. Ramana Murty ◽  
E. Butler ◽  
J. Pomeroy ◽  
B.H. Cooper ◽  
...  
Keyword(s):  
Scanning Tunneling Microscope ◽  
Ion Irradiation ◽  
Ion Beam ◽  
Normal Incidence ◽  
Scanning Tunneling ◽  
Layer By Layer ◽  
X Ray Diffraction ◽  
Tunneling Microscopy ◽  
X Ray ◽  
Glancing Angle

ABSTRACTUsing Scanning Tunneling Microscopy(STM) and X-ray diffraction(XRD), we have studied the development of surface roughness on Au(111) during 500eV Ar+ ion irradiation at different angles. During normal incidence erosion the surface roughens and pattern formation occurs. The surface morphology is a mixture of mounds and pits superimposed onto a larger structure of channels and valleys. The characteristic spacing between features grows with a power law behavior t27, where t is the amount of time the sample was irradiated, in agreement with previous measurements[l]. At glancing angles, erosion proceeds smoothly, but not in layer-by-layer fashion. Finally, a combination of glancing angle and normal incidence erosion is used to create a rippled morphology

scholarly journals Initial Interaction of Crystalline Al/Amorphous Si Bilayer during Annealing

2004 ◽  
Vol 808 ◽  
Author(s):  
Yonghao Zhao ◽  
Jiangyong Wang ◽  
Eric J. Mittemeijer
Keyword(s):  
Auger Electron ◽  
Focused Ion Beam ◽  
Imaging Techniques ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
X Ray ◽  
Initial Interaction ◽  
Magnetron Sputter ◽  
Amorphous Si ◽  
Sputter Deposited

ABSTRACTInitial interaction of a magnetron sputter deposited Al(100 nm, {111} fibre textured)/Si(150 nm, amorphous) bilayer, induced by isothermally annealing at 523 K for 60 min in a vacuum of 2.0×10−4 Pa, was studied by X-ray diffraction, Auger electron microscopy and focused-ion beam imaging techniques. Upon annealing, the crystalline Si had grown into the grain boundaries of the Al layer with a {111} texture, a crystallite size of approximate 12 nm and a tensile stress of +138 MPa. Simultaneously, the Al grains had grown into the Si layer from the original interface of the a-Si and Al sublayers with the lateral grain growth. The stress parallel to the surface of the Al layer had changed from +27 MPa to +232 MPa after annealing.

Synthesis of Nanodimensional TiO2 Thin Films

2008 ◽  
Vol 8 (8) ◽  
pp. 4231-4237 ◽  
Author(s):  
Madhavi Thakurdesai ◽  
T. Mohanty ◽  
J. John ◽  
T. K. Gundu Rao ◽  
Pratap Raychaudhuri ◽  
...  
Keyword(s):  
Thin Films ◽  
Ion Beam ◽  
Anatase Phase ◽  
Blue Shift ◽  
X Ray Diffraction ◽  
Tio2 Thin Films ◽  
Force Microscopy ◽  
Atomic Force ◽  
Glancing Angle ◽  
Photochromic Devices

Nanodimensional TiO2 has wide application in the field of photocatalysis, photovoltaic and photochromic devices. In present investigation TiO2 thin films deposited by pulsed laser deposition method are irradiated by 100 MeV Ag ion beam to achieve growth of nanophases. The nanostructure evolution is characterized by atomic force microscopy (AFM). The phases of TiO2 formed after irradiation are identified by glancing angle X-ray diffraction and Raman spectroscopy. The particle radius estimated by AFM varies from 10–13 nm. Anatase phase of TiO2 is formed after irradiation. The blue shift observed in UV-VIS absorption spectra indicates the nanostructure formation. The shape and size of nanoparticles formed due to high electronic excitation depend upon thickness of the film.

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