Nanohardness Profiles Research Articles

Impact of Glow-Discharge Nitriding Technology on the Properties of 3D-Printed Grade 2 Titanium Alloy.

This study presents a comparative analysis of the corrosion resistance of nitrided layers on conventional Grade 2 titanium alloy and those produced by direct metal laser sintering (DMLS). Low-temperature glow-discharge nitriding of the tested materials was carried out using conventional glow-discharge nitriding (so-called nitriding at the cathode potential-TiN/CP) and with the use of an "active screen" (nitriding at the plasma potential-TiN/PP). The TiN + Ti2N + Ti(N) layers were characterized by their microstructure, nanohardness profile distribution, surface topography, and corrosion resistance. The reduction in the cathodic sputtering phenomenon in the process using the active screen allowed the creation of surface layers that retained the topography of the base material. The parameters of the glow-discharge treatment led to grain growth in the printed substrates. This did not adversely affect corrosion resistance. The corrosion resistance of nitrided layers on the printed titanium alloy is only slightly lower than that of layers on the conventional Grade 2 alloy. Iron precipitates at grain boundaries facilitate increased nitrogen diffusion, resulting in reduced nitrogen concentration in the surface layer, slight changes in corrosion potential values, and increased nitrogen concentration in the Ti(N) diffusion layer.

Silver-promoted ceramic conversion treatment of Ti6Al4V alloy and its mechanical performance

In this paper, the Ti6Al4V alloy surface was modified via ceramic conversion treatment (CCT) with or without a pre-deposited silver layer. After characterizing the surface morphologies, microstructure and phase constituents of the ceramic oxide layer formed at 620 °C, we investigated the surface hardness and the cross-sectional nano-hardness profile under the oxide layer. The static load-bearing capacity of the oxide layers was examined by applying discrete loads via a Vickers indenter and observing the indentations. A scratch test was used to evaluate the load-bearing capacity and the adhesion/cohesion of the oxide layers. The wettability of the surface changed due to the incorporation of silver and the change of surface morphology. Reciprocating friction and wear test was used to assess the tribological properties. Small and dispersed silver nanoparticles and clusters were found in the oxide layer of the Ag pre-deposited Ti6Al4V samples, and they had much better tribological properties in terms of reduced coefficient of friction and wear volume. With the assistance of silver, the efficiency of the CCT was significantly improved.

A spatially resolved analysis of dislocation loop and nanohardness evolution in proton irradiated Zircaloys

Proton irradiation is increasingly used as a surrogate for neutron irradiation, providing similar damage structures at significantly lower costs and less time compared to neutron irradiation. However, in contrast to neutrons, protons produce a depth dependent damage profile that incorporates a plateau region and a Bragg peak in the tens of microns region depending on the material and proton energy. Here we demonstrate that this depth dependent damage can be utilised to obtain new understanding about irradiation induced damage at different dose levels from a single sample by combining spatially resolved micro-beam synchrotron X-ray diffraction-based dislocation analysis and nanoindentation. For this purpose, and to study the damage evolution starting from very early stages, we have investigated microstructure evolution and hardening behaviour of Zircaloy-2 and Zircaloy-4 proton irradiated samples between 0.01 dpa and 17 dpa at 350 °C. The results highlight good agreements of SRIM-based damage depth predictions with irradiation-induced dislocation appearance and nanohardness. However, at even relatively low damage levels within the plateau region, dislocation line density and nanohardness profiles appear saturated across the entire irradiated region, even when the dpa levels differed significantly. When relating dislocation loop line densities to nanohardness, it was found that from a certain point hardness increased only very slightly with increasing line densities. This apparent discrepancy can be explained by a decreasing loop size for the highest line densities identified by from the diffraction line profile analysis and the application of a Dispersed Barrier Hardening model that relates obstacle strength to dislocation loop size.

Influence of Filler on the Microstructure, Mechanical Properties and Residual Stresses in TIG Weldments of Dissimilar Titanium Alloys

The influence of titanium alloy (Ti–5Al–2.5Sn) and commercially pure titanium (cpTi) as fillers on dissimilar pulsed tungsten inert gas weldments of Ti–5Al–2.5Sn/cpTi was investigated in terms of microstructure, mechanical/nano-mechanical properties, and residual stresses. A partial martensitic transformation was observed in the weldments for all the welding conditions due to high heat input. The microstructure evolved in the FZ/cpTi interfacial region was observed to be the most sensitive to the proportion of α stabilizer in the filler alloy. Furthermore, the addition of filler alloy improved the tensile properties and nano-mechanical response of the weld joint owing to the increased volume of metal in the weld joint. As compared to the Ti–5Al–2.5Sn wire, the use of cpTi filler wire proved to be better in terms of energy absorbed during tensile and impact tests, tensile strength and ductility of the dissimilar welds. An asymmetrical residual stresses profile was observed close to the weld centerline, with high compressive stresses on the Ti–5Al–2.5Sn side for both the weldments obtained with and without filler wires. This was attributed to mainly the low thermal conductivity of Ti–5Al–2.5Sn. The presence of residual stresses also influenced the nano-hardness profile across the weldments.

Nanomechanical Response of Pulsed Tungsten Inert Gas Welded Titanium Alloy by Nanoindentation and Atomic Force Microscopy

Nanohardness and Effective Elastic Moduli were measured for pulsed-Gas Tungsten Arc Welded Ti-5Al-2.5Sn alloy using autogenous mode through nanoindentation and atomic force microscopy. Experiments were conducted using a Berkovich tip on nanoindentor with Berkovich tip and elliptical pile ups were measured using an Atomic Force Microscope. Nanohardness and effective elastic moduli were calculated in the base metal, heat affected zone and fusion zone of the weldments using different approaches namely Oliver–Pharr method, AFM analysis and work of indentation. A significant difference was observed in the nanomechanical response using these approaches which was attributed to the pile up morphology of the nano indents. The presence of residual stress in the weldments also significantly influenced the nanohardness profile across the weld joint. The present research suggested that the work of indentation is most suitable for assessment of nanomechanical properties of Ti-5Al-2.5Sn alloy weldments among the three techniques studied in this investigation.

Hardness and wear behaviour of electroless Ni–B coatings

Depth-dependent hardness variation of dimethylamine borane-reduced electroless Ni–5 wt-%B deposits has been examined using the nanoindentation technique. The deposits were characterised using ICP-OES, FESEM, XRD and DSC for evaluating the composition, morphology, structure and phase transformation behaviour, respectively. Coatings were also analysed for hardness and wear resistance. The surface of the as-plated deposit exhibits a typical nodular morphology. DSC traces show the presence of a single exothermic peak at 313°C conforming to its phase transformation. X-ray diffraction pattern of as-prepared deposit contains a mixture of amorphous and sharp microcrystalline nickel peaks. Heat-treated coating exhibits improved hardness and wear resistance. Depth-dependent nanohardness profile of as-deposited film neither obeys Nix–Gao nor the Lam–Chong model of indentation.

Compound technology of manufacturing and multiple laser peening on microstructure and fatigue life of dual-phase spring steel

The present work proposes an advanced double quenching and tempering heat treatment based laser surface modification process of dual-phase spring steel. Multiple laser peening without coating process utilized the decarburized surface as the protective layer for the further cold working process. The electron backscattering diffraction analysis on crystallographic orientation of individual grains and phase map exhibits a perfect dual-phase steel. Also, the high resolution transmission electron microscopic study explains the high strain induced microstructural grain refinement features and plastic deformation behaviors. The laser peening technique taking an advantage that it induces a large and high magnitude compressive residual stress with good thermal stability. The micro and nano-hardness profile provides better surface and sub-surface mechanical properties. The controlled average surface roughness is achieved in this course of work. The stress-strain characteristics on tensile properties are analyzed through the pre-fatigued specimens. The fully reversed high cycle fatigue test indicates that the current laser peening has substantially improves the fatigue life of the specimens.

In vitro Induction of Residual Caries Lesions in Dentin: Comparative Mineral Loss and Nano-Hardness Analysis

Artificially inducing dentinal lesions mimicking those remaining after selective excavation should allow to investigate the effects and limits of such selective excavation, for example regarding the mechanical properties of treated teeth or the remineralisation of sealed residual lesions. Such analyses might otherwise be limited by the variability of natural lesions or ethical and practical concerns. This study compared different demineralisation protocols for their suitability to induce lesions similar to natural residual caries. Twelve natural deep lesions were excavated until leathery dentin remained, and analysed for their mineral loss (ΔZ), lesion depth (LD), mineral loss ratio (R), the slope of the mineral gradient and their nano-hardness profile. Artificial lesions were induced using four different demineralisation protocols (acetic acid pH = 4.95; 0.1 <smlcap>M</smlcap> lactic acid gel pH = 5.0; 0.5 <smlcap>M</smlcap> ethylenediaminetetraacetic acid pH = 7.2; Streptococcus mutans biofilms) and their depths monitored over different demineralisation times. Lesions with depths most according to those of natural lesions were analysed using transversal microradiography. Lesions induced by acetic acid solution did not significantly differ with regards to LD, ΔZ, R and mineral profile. Seven dentin specimens were subsequently submitted to a moderately acidic (pH = 5.3) methylhydroxydiphosphonate-buffered acetate solution for 12 weeks. Natural and artificial residual lesions were similarly deep (mean ± SD: LD = 626 ± 212 and 563 ± 88 µm), demineralised (R = 19.5 ± 4.7 and 29.8 ± 4.1%), showed a flat and continuous mineral gradient (slope = 0.10 ± 0.05 and 0.13 ± 0.06 vol%/µm) and did not significantly differ regarding their nano-hardness profile. The described protocol induces lesions with mineral content and mechanical properties similar to natural residual lesions.

Nanostructuring of surfaces of metalloceramic and ceramic materials by electron-beams

An electron-emitting source generating a low-energy beam measuring 1–3 cm in diameter, with current up to 300 A, pulse duration within 50–200 µs, and pulse repetition frequency up to 10 Hz is investigated in a gas-filled diode with a mesh plasma cathode at the accelerating voltage up to 25 kV. The beam is transported in a longitudinal pulsed magnetic field to a distance of up to 30 cm towards the region of its interaction with a solid. For the current densities up to 100 A/cm2, it provides the power density as high as 10–100 J/cm2 sufficient to melt surfaces of metals, alloys, and composite (metalloceramic) materials within one or a few pulses. This makes this beam useful for modification of material surfaces and articles made thereof. Using the methods of optical, scanning and diffraction electron microscopy, by building micro-and nanohardness profiles, and via identification of the treated surface roughness, the phase composition and the substructure state of the materials subjected to pulsed low-energy e-beam of sub-millimeter durations are investigated. Formation of submicro-and nanocrystalline multi-phase structure is observed, which ensures a multiple increase in physico-mechanical and tribological characteristics of the treated material.

Plasma nitridation of a novel Ni–10.8 wt.%Cr nanocomposite

A Ni–10.8Cr nanocomposite (by wt.%), consisting of nanocrystalline Ni matrix (mean grain size: 60 nm) and dispersed Cr nanoparticles (mean particle size: 42 nm), has been synthesized by nanocomposite electrodeposition. The unique structure causes the nanocomposite to form a double-layered nitrided zone during plasma nitridation at 560 °C for 10 h. The outer layer (∼50 μm thick) precipitates nanometer-sized CrN (<100 nm), which increased in size but decreased in number with increasing nitridation depth (following Böhm–Kahlweit’s mode). The inner layer (∼5 μm thick) exhibits larger-coarsened nitride precipitates (100–200 nm) which almost link together. The greatly enhanced nitriding kinetics in the nanocomposite compared to a compositionally similar but microstructurally different Ni–10Cr alloy (mean grain size: 30 μm) is mainly associated with the fact that the numerous grain boundaries dramatically increase the nitrogen permeability, according to the treatment using a classical Wagner’s approach. The nanohardness profile in relation to the microstructure of the nitrided zone in the nanocomposite has also been investigated.

1129 ヒト歯象牙質のナノインデンテーション試験による力学的特性の評価(S11-1 計測と力学-生体への応用(1),S11 計測と力学-生体への応用)

Mechanical understanding of dentin properties of is important for development of new dental materials, and is prerequisite to reveal the function and mechanisms of human hard tissues. In this study, nanoindentation test with specimens from permanent incisor teeth were used to evaluate the gradients in the overall mechanical properties, including nano-hardness and elastic modulus of a human dentin. It is shown from the results that decreasing gradient mechanical properties seems to be existed from crown to root of apex in incisor dentin. The elastic modulus and nano-hardness profiles were characterized by remarkable S-shaped curve for root dentin.

Depth profile of nitrogen concentration and nano-hardness in nitrogen implanted Zr at RT and at 600 °C

To study the property changes of Zr induced by high dose nitrogen implantation at RT and at 600 °C, the depth profiles of nanohardness were measured and compared with those of nitrogen concentration and chemical states of nitride phase. The implantation was performed with 100 keV N + 2 ions and doses from 1×10 16 to 1×10 18 N/cm 2. The nanohardness was measured by an ultra micro indentation tester. The nitrogen depth profile was measured by NRA using 15 N (α,γ) 12C reaction and RBS, Depth dependence of chemical state was measured by XPS combined with Ar sputtering. Dose and temperature dependence of the crystalline structure were measured by glancing angle XRD. There was no difference in the XPS spectra between RT and 600 °C, and the spectra indicated that ZrN was formed at the depth where nitrogen existed. Since the heat of formation of ZrN is rather high, the depth profile of the implanted nitrogen in Zr was hardly changed up to 600 °C. But the XRD patterns showed the increase of crystalline nitride phase with the increase of implantation and annealing temperatures. From the dose and temperature dependence of nanohardness profile, the hardness increase by low dose implantation around 1×10 17 ions/cm 2 at both RT and 600 °C is attributed to point defects and interstitial hardening and the increase by high dose implantation above a dose around 5×10 17 ions/cm 2 at 600 °C is attributed to the formation of ZrN phase.