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.

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.

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.

Preparation of Bioactive Titanium Film via Anodic Oxidation in Agitation Condition

2016 ◽  
Vol 840 ◽  
pp. 220-224
Author(s):  
Te Chuan Lee ◽  
Mohd Hafifi Hafizat Mazlan ◽  
Mohamad Imran Abbas ◽  
Hasan Zuhudi Abdullah ◽  
Maizlinda Izwana Idris
Keyword(s):  
Oxide Layer ◽  
Surface Properties ◽  
Anodic Oxidation ◽  
Disodium Salt ◽  
Agitation Speed ◽  
Ion Diffusion ◽  
Titanium Film ◽  
Protective Oxide ◽  
Single Lens ◽  
Titanium Foils

Anodic oxidation is a well-established surface modification method which combines electric field driven metal and oxygen ion diffusion to produce protective oxide layer on metals. This method has been widely used to modify the surface properties of titanium and its alloy. This present study aims to investigate the effect of agitation speed on the surface properties of anodised titanium. At first, the high purity titanium foils were anodised in mixture of 0.04 M β-glycerophosphate disodium salt pentahydrate (β-GP) and 0.4 M calcium acetate monohydrate (CA) at 350 V and 30 mA.cm-2 for 10 minutes at different agitations speed (300 rpm - 1500 rpm). Next, surface properties of anodised titanium were characterised by digital single-lens reflex camera (DSLR camera), field emission scanning electron microscopy (FESEM) and glancing angle X-ray diffractometer (GAXRD). At lower agitation speed (≤ 900 rpm), surface of anodised titanium covered by small donut-shaped pores. With increasing of agitation speed (≥ 1100 rpm), the oxide layer became more porous and covered by larger donut-shaped pores. Rutile TiO2 peaks were detected at agitation speed more than 1100 rpm. Agitation condition is believed to be an effective method to enhance the surface properties of anodised titanium for biomedical applications.

scholarly journals Change in the Microstructure of Ferritic Stainless Steel with Surface Roughness and the Number of Thermal Cycles

2021 ◽  
Author(s):  
Myoung Youp SONG
Keyword(s):  
Surface Roughness ◽  
Stainless Steel ◽  
Oxide Layer ◽  
Ferritic Stainless Steel ◽  
Exposure Time ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Thermal Cycles ◽  
Total Oxygen ◽  
Oxygen Exposure

One of the candidates for metallic interconnects of solid oxide fuel cells is ferritic stainless steel, Crofer 22 APU. Ferritic stainless steel Crofer 22 APU specimens with different surface roughness were prepared by grinding with SiC powder papers of various grits and then thermally cycled in air. Variation in the microstructure of the samples having different roughness with thermal cycling was investigated. Polished Crofer 22 APU specimens after three and five thermal cycles had relatively flat oxide layers with thicknesses of about 13.8 and 17.9 μm, respectively. Micrographs of a trench made by milling with FIB (focused ion beam) for a Crofer 22 APU specimen ground with grit 80 SiC powder paper after 8 thermal cycles (total oxygen exposure time of 200 h at 1073 K), captured by ESB (energy selective back-scattering) and SE2 (type II secondary electrons), showed that the surface of the sample was very coarse and its oxide layer was undulated. In the oxide layer, the phase of the sublayer was Cr2O3, and that of the top layer was (Cr, Mn)3O4 spinel. The surface of the sample ground with grit 80 SiC powder paper was very rough after 60 thermal cycles (total oxygen exposure time of 1500 h at 1073 K). The polished Crofer 22 APU is a better applicant to an interconnect of SOFC than those with rougher surfaces.

Focused ion beam strategy for nanostructure milling in doped silicon oxide layer for light trapping applications

Vacuum ◽  
2014 ◽  
Vol 99 ◽  
pp. 135-142 ◽  
Author(s):  
V. La Ferrara ◽  
P.M. Aneesh ◽  
P. Delli Veneri ◽  
L.V. Mercaldo ◽  
I. Usatii ◽  
...  
Keyword(s):  
Oxide Layer ◽  
Focused Ion Beam ◽  
Silicon Oxide ◽  
Light Trapping ◽  
Ion Beam ◽  
Silicon Oxide Layer ◽  
Doped Silicon

Atom Probe Tomography of the Oxide Layer of an Austenitic Stainless CrMnN-Steel

2021 ◽  
Vol 58 (5) ◽  
pp. 264-281
Author(s):  
S. Monschein ◽  
R. Schnitzer ◽  
R. Fluch ◽  
C. Turk ◽  
C. Hofer
Keyword(s):  
Oxide Layer ◽  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Sample Surface ◽  
Atom Probe ◽  
Passive Layer ◽  
Silver Layer ◽  
Voltage Mode ◽  
Pulsed Voltage

Abstract This work aimed at developing a methodology for examining the naturally grown passive layer of a thickness of just a few nanometers of an austenitic CrMnN steel by means of atom probe tomography and gaining knowledge on the structure of this alloy’s passive layer. The sample surface was ground, polished, cleaned, degreased, electrolytically polished, and oxidized in air to produce a reproducible passive layer. The oxide layer was subsequently coated with a silver layer of a thickness of 3 μm. The silver layer protects the oxide layer during the preparation of the atom probe tips in the focused ion beam microscope and the alignment of the tip in the atom probe. The samples were measured in the atom probe’s pulsed-voltage mode. The findings show that an enrichment of oxygen, molybdenum, nitrogen, and chromium and a depletion of manganese, nickel, and iron occur in the area of the passive layer.

Study on the Variation in Microstructure of a Ferritic Stainless Steel with Surface Roughness and Thermal Cycling in Air

2021 ◽  
Vol 21 (8) ◽  
pp. 4372-4382
Author(s):  
Myoung Youp Song ◽  
Daniel R. Mumm ◽  
Young Jun Kwak
Keyword(s):  
Stainless Steel ◽  
Oxide Layer ◽  
Ferritic Stainless Steel ◽  
Exposure Time ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Thermal Cycles ◽  
Total Oxygen ◽  
Oxygen Exposure ◽  
Better Than

A ferritic stainless steel, Crofer 22 APU, is one of candidates for metallic interconnects of solid oxide fuel cells. Ferritic stainless steel Crofer 22 APU specimens with different surface roughnesses were prepared by grinding with SiC powder papers of various grits and were then thermally cycled. Polished Crofer 22 APU specimens after one thermal cycle and five thermal cycles had relatively straight oxide layers with similar thicknesses of 30 μm, suggesting that after one cycle (total oxygen exposure time of 100 h at 1073 K), the oxidation does not progress. Micrographs of a trench made by milling with the FIB (focused ion beam) for a Crofer 22 APU specimen rubbed with grit 80 SiC powder paper after 8 thermal cycles (total oxygen exposure time of 200 h at 1073 K), captured by ESB, InLens, and SE2, showed that the surface of the sample was very coarse and its oxide layer was undulated. In the oxide layer, the phase of the sublayer was Cr2O3, and that of the top layer was (Cr, Mn)3O4 spinel. The sample ground with grit 80 SiC powder paper after 60 thermal cycles (total oxygen exposure time of 1500 h at 1073 K) was very coarse. Some ridges were quite straight and continuous. After 20 and 40 thermal cycles, ASR (area specific resistance) decreased as the number of grit of the SiC powder paper increased, suggesting that the polished Crofer 22 APU is better than those with rougher surfaces for application as an interconnect of SOFC.

Nanocomposite Polyurethane Foams Via POSS Blends

2002 ◽  
Vol 733 ◽  
Author(s):  
Brock McCabe ◽  
Steven Nutt ◽  
Brent Viers ◽  
Tim Haddad
Keyword(s):  
High Temperature ◽  
Sample Preparation ◽  
Room Temperature ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Polyurethane Foams ◽  
Development Projects ◽  
Polymer Systems ◽  
Polyurethane Resin ◽  
Military Development

AbstractPolyhedral Oligomeric Silsequioxane molecules have been incorporated into a commercial polyurethane formulation to produce nanocomposite polyurethane foam. This tiny POSS silica molecule has been used successfully to enhance the performance of polymer systems using co-polymerization and blend strategies. In our investigation, we chose a high-temperature MDI Polyurethane resin foam currently used in military development projects. For the nanofiller, or “blend”, Cp7T7(OH)3 POSS was chosen. Structural characterization was accomplished by TEM and SEM to determine POSS dispersion and cell morphology, respectively. Thermal behavior was investigated by TGA. Two methods of TEM sample preparation were employed, Focused Ion Beam and Ultramicrotomy (room temperature).

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