Investigations on the mechanical properties and microstructure of dissimilar cp-titanium and AISI 316L austenitic stainless steel continuous friction welds

Friction welding process is a solid state joining process that produces a weld under the compressive force contact of one rotating and one stationary work piece. In this study, the friction welding of dissimilar joints of AISI 316L stainless steel and cp-titanium is considered. The optical, scanning electron microscopy studies of the weld were carried out. Moreover, the X-ray diffraction analysis was performed. The integrity of welds was achieved by the micro hardness and tensile tests. The fracture surface was examined by the scanning electron microscopy. The study showed that the magnitude of tensile strength of the dissimilar welded specimen was below that of the titanium base material if preheating was not applied at the interface. The high weld tensile strength was achieved by preheating the 316L stainless steel material to 700 °C, smoothing and cleaning of the contact surfaces. Results illustrated that in dissimilar joints, different phases and intermetallic compounds such as FeTi, Fe₂Ti, Fe₂Ti₄O, Cr₂Ti and sigma titanium phase were produced at the interface. The presence of brittle intermetallic compounds at the interface resulted in degradation of mechanical strength which in turn led to premature failure of joint interface in the service condition. Preheating caused to produce oxide layer at the interface which was harmful for bonding. The oxide layer could be eliminated by applying pressure and smoothing the surface. Results of hardness tests illustrated that the high hardness was occurred in the titanium side adjacent to the joint interface. Moreover, the optimum operational parameters were obtained in order to achieve the weld tensile strength greater than the weak titanium material.     

Some properties of boronized layers on steels with direct diode laser

Boronized layer on steel is known to be formed by thermal diffusion of boron into the surface of steel improving corrosion-erosion resistant properties. Boronizing is carried out at temperatures ranging from 800 °C to 1050 °C and takes from one to several hours. There is one problem in this process, however, that the structure and properties of the base material are influenced considerably by the high temperature and long time of treatment. In order to avoid the aforementioned drawbacks of pack boronizing and laser-assisted boronizing, a better way is to activate the pack boronizing media and the workpiece with a high density power. The laser boronizing processes do not change the properties of the base material. In this study, the effect of laser characteristics was examined on the laser boronizing of carbon steel. After laser boronizing, the microstructure of the boride layer was analysed with an optical microscope and X-ray diffractometer (XRD). The mechanical properties of borided layer are evaluated using Vickers hardness tester and sand erosion tester. Results showed that the boride layer was composed of FeB and Fe₂B with thickness ranging 200-300 μm. The laser boronizing process did not change the properties of the base material.     

One-step synthesis of petal-like apatite/titania composite coating on a titanium by micro-arc oxidation

Petal-like apatite/titania (TiO₂) coating was prepared on commercially pure titanium (Ti) by micro-arc oxidation in electrolyte containing calcium and phosphate for the first time. The surface morphology, crystalline structure, chemical composition and binding state of the apatite/TiO₂ composite coating were characterized. The coating consists of a double-layer (apatite layer and TiO₂ layer) structure. The average thickness of the inner TiO₂ layer and the outer apatite layer is about 6 μm and 16 μm respectively. The outer apatite layer is porous and exhibits petal-like pattern. The apatite layer consists of hydroxyapatite (HA) and carbonate-apatite and the inner TiO₂ layer consists of anatase and rutile.     

Duplex surface treatment of AISI 1045 steel via plasma nitriding of chromized layer

In this work AISI 1045 steel were duplex treated via plasma nitriding of chromized layer. Samples were pack chromized by using a powder mixture consisting of ferrochromium, ammonium chloride and alumina at 1273 K for 5 h. The samples were then plasma-nitrided for 5 h at 803 K and 823 K, in a gas mixture of 75%N₂ + 25%H₂. The treated specimens were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) analysis and Vickers micro-hardness test. The thickness of chromized layer before nitriding was about 8 μm and it was increased after plasma nitriding. According to XRD analysis, the chromized layer was composed of chromium and iron carbides. Plasma nitriding of chromized layer resulted in the formation of chromium and iron nitrides and carbides. The hardness of the duplex layers was significantly higher than the hardness of the base material or chromized layer. The main cause of the large improvement in surface hardness was due to the formation of Cr_xN and Fe_xN phases in the duplex treated layers. Increasing of nitriding temperature from 803 to 823 K enhanced the formation of CrN in the duplex treated layer and increased the thickness of the nitrided layer.     

Titanium-oxide interface structures formed by degassing and anodization processes

High-resolution electron microscopy was used to investigate two types of titanium-oxide interface structures. The first type was generated by thermal oxidation during the degassing process, which is one step in the process of porcelain-fused-to-metal systems. The thermal oxidation was performed for 1 min at a temperature of 1073 K in a porcelain furnace under a reduced pressure at 27 hPa. Columnar and granular rutile oxide formed on the titanium, and the surface oxide layer was almost 1 μ m thick. On an atomic scale, the crystal size of the rutile adjacent to the interface decreased about 10 nm. In addition, a very thin transitional layer 2–3 nm thick formed at the titanium-oxide interface. The crystal structure of the thin layer seemed to be the T{i}O phase with a NaCl-type structure. The interface between the hcp titanium and T{i}O phases was coherent through the close-packed planes ((0 0 0 2)_hcp and (1 1 1)_TiO). Partial coherency was observed at the interface between the T{i}O and T{i}O₂ phases. The second type of titanium-oxide interface was generated by anodization on a screw-type titanium implant. The morphology of the surface suggested that the titanium implant had been treated by spark anodization. The surface oxide, which was estimated to be about 10 μ m thick, was a mixture of the anatase-type T{i}O₂ phase and the amorphous phase. The crystal size of the anatase varied from less than 10 nm to more than 100 nm. A phosphate anion was concentrated in the amorphous phase. Between the surface oxide and the titanium base, macroscopic defects like cracks and voids were observed. Microscopic observation could not confirm the formation of a clear interface and lattice coherency between the titanium and oxide as a result of the degassing process.     

Corrosion behaviour of single (Ti) and duplex (Ti–TiO2) coating on 304L stainless steel in nitric acid medium

Sputter deposited single titanium (Ti) layer, and duplex Ti–TiO₂ coating on austenitic type 304L stainless steel (SS) was prepared, and the corrosion performance was evaluated in nitric acid medium using surface morphological and electrochemical techniques. Morphological analysis using atomic force microscope of the duplex Ti–TiO₂ coated surface showed minimization of structural heterogeneities as compared to single Ti layer coating. The electrochemical corrosion results revealed that, titanium coated 304L SS showed moderate to marginal improvement in corrosion resistance in 1 M, and 8 M nitric acid, respectively. Duplex Ti–TiO₂ coated 304L SS specimens showed improved corrosion resistance as compared to Ti coating from dilute (1 M) to concentrated medium (8 M). The percentage of protection efficiency for base material increases significantly for duplex Ti–TiO₂ coating as compared to single Ti layer coating. The oxidizing ability of nitric acid on both the coatings as well as factors responsible for improvement in protection efficiency are discussed and highlighted in this paper.     

Fracture behavior of nano-layered coatings under tension

The fracture of brittle/ductile multilayers composed of equal thicknesses of Si and Ag layers evaporated on a thick substrate is studied with the aid of a four-point bending apparatus. The system variables include individual layer thickness (2.5 to 30 nm), total film thickness (0.5 to 3.5 μm) and substrate material (polycarbonate, aluminum alloy and hard steel). The fracture is characterized by transverse cracks that proliferate with load. The crack initiation strain ε_i is virtually independent of total film thickness and substrate material while increasing with decreasing layer thickness h, to a good approximation as ε_i ~ 1/h^1/2. At higher strains, film debonding and buckling are evident.The fracture conditions are determined with the aid of a 2D finite element analysis incorporating the inelastic response of the interlayer. A fracture scenario consisting of tunnel cracking in the brittle layers followed by cracking in the interlayers is shown to be capable of predicting the observed increase in crack initiation strain with decreasing layer thickness. To realize this benefit the interlayer must be compliant and tough to force tunnel cracking in the brittle layers. The explicit relation for the crack initiation strain obtained from the analysis can be used to assess fracture toughness and improve damage tolerance in nanoscale layered structures.     

Properties of pulsed laser deposited fluorinated hydroxyapatite films on titanium

Fluorinated hydroxyapatite coated titanium was investigated for application as implant coating for bone substitute materials in orthopaedics and dentistry. Pulsed laser deposition technique was used for films preparation. Fluorinated hydroxyapatite target composition, Ca₁₀(PO₄)₆F_1.37(OH)_0.63, was maintained at 2 J/cm² of laser fluence and 500-600 °C of the substrate temperature. Prepared films had a compact microstructure, composed of spherical micrometric-size aggregates. The average surface roughness resulted to be of 3 nm for the film grown at 500 °C and of 10 nm for that grown at 600 °C, showing that the temperature increase did not favour the growth of a more fine granulated surface. The films were polycrystalline with no preferential growth orientation. The films grown at 500-600 °C were about 8 μm thick and possessed a hardness of 12-13 GPa. Lower or higher substrate temperature provides the possibility to obtain coatings with different fine texture and roughness, thus tayloring them for various applications.     

Initiated chemical vapor deposition of a siloxane coating for insulation of neural probes

Recent advances in the field of neuroprosthetics have brought the possibility of human utilization into the near term. However, current implant coating chemistries require thicknesses of ~ 25 μm in order to provide the required electrical insulation, significantly increasing the diameter of the neural probe shanks and resulting surgical damage upon implantation. In this work, a novel biopassivation coating is created through initiated chemical vapor deposition (iCVD) of trivinyl-trimethyl-cyclotrisiloxane. The resulting material is a highly crosslinked organosilicon polymer matrix which is synthesized directly on the surface of the substrate. This material possesses an electrical resistivity which allows for a coating thickness on the order of only 5 μm. The material has also been demonstrated to retain its electrical properties in a simulated biological environment for over 3 years.     

Tribology of ultra high molecular weight polyethylene film on Si substrate with chromium nitride, titanium nitride and diamond like carbon as intermediate layers

This paper presents tribological studies on composite films consisting of different intermediate hard layers (chromium nitride (CrN), titanium nitride (TiN) and diamond like carbon (DLC)) on Si substrate followed by soft ultra high molecular weight polyethylene (4-5 μm thick) as the top layer. The tribological properties of the composite films were evaluated on a ball-on-disc tribometer (composite film sliding against a 4 mm diameter Si₃N₄ ball) at a normal load of 40 mN and a linear speed of 0.052 m/s. The wear durability of the composite films increases with increasing hardness of the intermediate layers. The composite film with harder intermediate layers (TiN with 24 GPa and DLC layers with 57 GPa and 70 GPa of hardness) provides the best tribological performance with more than 300,000 cycles of sliding when the experiments were stopped. The critical loads of scratching correlate with the wear performances of the composite films. Application of only a few nanometer overcoat of perfluoropolyether on the most wear resistant composite films can further increase the wear lives (more than one million cycles) even at a higher normal load of 70 mN.     

Nature in corrosion-erosion surface for [TiN/TiAlN]n nanometric multilayers growth on AISI 1045 steel

The aim of this work is to characterize the electrochemical behavior of [TiN/TiAlN]n multilayer coatings under corrosion-erosion condition. The multilayers with bilayer numbers (n) of 2, 6, 12, and 24 and/or bilayer period (Λ) of 1500 nm, 500 nm, 250 nm, 150 nm and 125 nm were deposited by magnetron sputtering technique on Si (100) and AISI 1045 steel substrates. Both, the TiN and the TiAlN structures for multilayer coatings were evaluated via X-ray diffraction analysis. Mechanical and tribological properties were evaluated via nanoindentation measurements and scratch test respectively. Silica particles were used as abrasive material on corrosion-erosion test in 0.5 M of H₂SO₄ solution at impact angles of 30° and 90° over surface. The electrochemical characterization was carried out using polarization resistance technique (Tafel), in order to observe changes in corrosion rate as a function of the bilayer number (n) or the bilayer period (Λ) and the impact angle. Corrosion rate values of 9115 μm y for uncoated steel substrate and 2615 μm y for substrate coated with n = 24 (Λ = 125 nm) under an impact angle of 30° were found. On the other hand, for an impact angle of 90° the corrosion rate exhibited 16401 μm y for uncoated steel substrate and 5331 μm y for substrate coated with n = 24 (Λ = 125 nm). This behavior was correlated with the curves of mass loss for both coated samples and the surface damage was analyzed via scanning electron microscopy images for the two different impact angles. These results indicate that TiN/TiAlN multilayer coatings deposited on AISI 1045 steel represent a practical solution for applications in corrosive-erosive environments.     

Effect of BN grain size on microstructure and mechanical properties of the ZrB2–SiC–BN composites

ZrB₂–20 vol.%SiC composites containing 10 vol.% h-BN particles (ZSB) with average grain sizes ranging from 1 μm to 10 μm were hot-pressed. The fracture toughness of the ZSB composites was higher than reported results of monolithic ZrB₂ (2.3–3.5 MPa m^1/2) and SiC particle reinforced ZrB₂ composites (4.0–4.5 MPa m^1/2). The improvement in the fracture toughness of the ZSB composites was due to the high aspect ratio of h-BN and weaker interface bonding, which could enhance crack deflection and stress relaxation near the crack-tip. Compared with the flexural strength of the ZrB₂–SiC composites, the reduction in the flexural strength of the ZSB composites was attributed to the weaker interface bonding and the lower relative density. Furthermore, improvement in toughness and the reduction in the strength were valuable to improve the thermal shock resistance of the ZSB composites. The ΔT_c of ZSB5 material is 400 °C which is higher than ZrB₂–20%SiC and ZrB₂–15%SiC–5%AlN.     

Poly-silicon thin films by aluminium induced crystallisation of microcrystalline silicon

Al-induced crystallisation of microcrystalline Si thin films prepared by electron cyclotron resonance plasma-enhanced chemical vapour deposition (ECR-PECVD) on glass and SiO₂ coated Si wafers has been studied. The starting structure was substrate/μc-Si/Al. Annealing this structure in the temperature range 370-520 °C, immediately following deposition of the Al layer, resulted in successful layer exchange and the formation of a substrate/Al+Si layer/poly-Si geometry. The top poly-Si layer exhibited grain sizes generally in the range ∼2-6 μm, although larger grains were also sparsely present. The films did not exhibit any appreciable degree of preferred orientation. The surface roughness was relatively high with a R_a value of ∼20 nm.     

Development of highly porous titanium scaffolds by selective laser melting

The selective laser melting (SLM) of the TiH₂-Ti blended powder was performed in the present work. Porous titanium scaffolds characterized by high porosity (∼ 70%), interconnected Ti walls and open porous structures with macroscopic pores (in a range of ∼ 200 to ∼ 500 μm) were successfully prepared at a laser power of 1000 W and a scan speed of 0.02 m/s. The effects of componential and processing conditions in terms of TiH₂ content and scan speed on the microstructural development of porous titanium (porosity and pores size) were investigated. Reasonable mechanisms for pores formation during SLM apart from microstructural evolutions were proposed.     

Morphological, structural and optical properties of thin SiC layer growth onto silicon by pulsed laser deposition

Crystalline silicon carbide thin layers were grown on a p-type Si(1 0 0) substrate by pulsed laser deposition (PLD) using KrF excimer laser at λ=248 nm from a 6H-SiC hot-pressed target. The target “SiC” used to elaborate our SiC films is realized from a mixture of 1SiO₂ with 3C (carbon) “1SiO₂+3C” heated in an oven at 2500 °C (the target was a hot-pressed material and supplied by Goodfellow). The morphological, structural and optical properties of SiC layers were investigated by scanning electronic microscopy (SEM), high-resolution X-ray diffraction (XRD), secondary ion mass spectrometry (SIMS) and UV-visible spectrophotometer. XRD analysis of the target showed that this latter is a hexagonal structure (6H-SiC). The XRD pattern shows that a 1.6 μm crystalline SiC layer was formed. In addition, a SIMS analysis gives a ratio Si/C of the thin SiC layer around 1.15 but the ratio Si/C of the target was found equal to 1.06, whereas one should have 1.0. This is due to the degree of the sensitivity of the SIMS technique and due to the higher ionization efficiency of Si compared to C atoms, all these which give different ratios. It is known that the PLD technique reproduces the same macroscopic property (optical, mechanical, structural, etc.) of the target. An optical gap (E_Gap) of the SiC layer of about 2.51 eV was obtained by reflectance measurement. Finally, a crystalline thin SiC layer of 1.6 μm was elaborated using PLD method at low-temperature deposition.     

Fast release process of metal structure using chemical dry etching of sacrificial Si layer

An ultra-fast removal process of a silicon sacrificial layer for the selective release of a metal structure on a Si substrate was studied, which uses a chemical dry etching method. The chemical dry etching of a Si layer was performed in an NF₃ remote plasma with the direct injection of additive nitric oxide (NO) gas. When the NO gas was injected into the chamber into which F radicals were supplied from a remote plasma source using NF₃ input gas, the silicon layer was removed selectively and the metal structure could be released easily. It was found that the etch rate on the sidewall (up to ≅ 18.7 μm/min for an opening width of 100 μm) and the bottom (up to ≅ 24.5 μm/min for an opening width of 100 μm) depends on the NO/(NO + Ar) gas flow ratio, time duration, and opening width. The developed dry etching process could be used to release a Ni structure with near infinite selectivity in a very short time. The process is well suited for fabricating various devices which require a suspended structure, such as in radio-frequency microelectromechanical system switches, tunable capacitors, high-Q suspended inductors and suspended-gate metal-oxide semiconductor field-effect transistors.     

Field emission characteristics of carbon nanofibers grown on copper micro-tips at low temperature

Carbon nanofibers (CNFs) were grown on copper micro-tips formed by electroplating. The nickel layer electroplated over the copper micro-tips was used as a catalyst. The CNFs were synthesized by using plasma-enhanced chemical vapor deposition (PECVD) of C₂H₂ and NH₃ at 480 °C. The copper micro-tips were formed by high current pulse electroplating, which played a significant role in characterizing our CNFs. The CNFs grown on the copper micro-tips showed outstanding field emission performance and stability, whose turn-on field, defined as one at the current density of 10 μA/cm², was 1.30 V/μm and the maximum current density reached 5.39 mA/cm² at an electric field of 4.9 V/μm.     

Ultrastructure of the bone-titanium interface in rabbits

The interface zone between cortical bone and threaded non-alloyed titanium implants inserted in the rabbit tibia for 12 months was examined by light and electron microscopy. The implants were removeden bloc with the perfusion-fixed surrounding bone and the undecalcified specimens were, after osmification, dehydrated and embedded in plastic resin (LR White). In ground sections (about 10 µm thick) cortical bone appeared to be in direct contact with the implant surface and the implants were thus osseointegrated. Sections for light microscopy (1 µm thick) and electron microscopy (40 nm to 0.5 µm) were prepared by using an electropolishing technique by which the bulk part of the metal was electrochemically removed and a fracture technique by which the implant was separated from the embedded tissue before sectioning. In the electropolished specimens an unmineralized zone, 2–10 µm wide, was observed at the interface. The interface zone contained osteoid-like tissue (densely packed collagen fibrils, osteocyte canaliculi) but in general no deposits of calcium mineral. This feature of the interface could not be observed in specimens prepared by the fracture technique, indicating that the electropolishing technique had induced serious artefacts, including decalcification of the interface bone. In sections prepared by the fracture technique, mineralized bone was present very close to the implant surface. No gradient of mineral was observed. A thin layer of amorphous material (100–200 nm wide) was present peripheral to the mineralized bone. An electron dense line about 100 nm wide was formed at the border between the mineralized bone and the amorphous layer. The dense layer had the same characteristics as the lamina limitans observed around osteocyte lacunae and canaliculi or the zone between areas of bone with different degree of mineralization.Our observations suggest that mineralized bone reached close to the surface of titanium implants inserted in the rabbit tibia for 12 months but that a direct contact is not established.     

Structural characterization of fluidized bed nitrided steels

The nitriding behaviour of 34CrAlNi7, 42CrMo4 and 40CrMnMoS86 steels was investigated nitrided in the fluidized bed processes. The nitriding processes were carried out at a temperature of 575 °C for treatment times of 6, 12 and 18 h. The nitrided samples were fully characterized using metallographic, microhardness and XRD techniques. Test results indicated that thickness of the compound layer on the steel surface changed in the range from 10 to 18 μm depending on steel type and treatment time, and γ′-Fe₄N and ε-Fe₂₋₃N formed in the compound layer. The hardness of the diffusion layer was over 1000 HV. Depending on the chemical composition of steels, the case depth ranged from 155 to 525 μm. Kinetics studies showed that the effective diffusion coefficients are 298×10⁻¹⁴, 525×10⁻¹⁴ and 68.8×10⁻¹⁴ m² s⁻¹, for 34CrAlNi7, 42CrMo4 and 40CrMnMoS86 steels, respectively. The fluidized bed process realizes the highest hardness of the case layer, 1095 HV, with fairly high growth rates, 27 μm/h.     

Investigation of inter-diffusion in bilayer GeTe/SnSe phase change memory films

A metal-chalcogenide layer, SnSe, is inserted between the memory layer GeTe and the top electrode to form a phase change memory cell. The GeTe layer exhibits ovonic threshold switching at a threshold field of ~ 110 V/μm. For subsequent implementation into applications and reliability, material inter-diffusion and sublimation are examined in bilayer phase change films of GeTe/SnSe. Transmission electron microscopy and parallel electron energy loss spectroscopy analyses reveal Sn migration to the GeTe layer, which is responsible for lowering the rhombohedral to cubic structural transformation temperature in GeTe. Incongruent sublimation of SnSe and GeTe is observed at temperatures higher than 500 °C. Severe volatilization of Se results in the separation of a metallic Sn phase. The use of Al₂O₃ as a capping layer has been found to mitigate these effects.