Nadimul Haque Faisal

Nanoindentation of polysilicon and single crystal silicon: Molecular dynamics simulation and experimental validation

This paper presents novel advances in the deformation behaviour of polycrystalline and single crystal silicon using molecular dynamics (MD) simulation and validation of the same via nanoindentation experiments. In order to unravel the mechanism of deformation, four simulations were performed: indentation of a polycrystalline silicon substrate with a (i) Berkovich pyramidal and a (ii) spherical (arc) indenter, and (iii and iv) indentation of a single crystal silicon substrate with these two indenters. The simulation results reveal that high pressure phase transformation (HPPT) in silicon (Si-I to Si-II phase transformation) occurred in all cases; however, its extent and the manner in which it occurred differed significantly between polycrystalline silicon and single crystal silicon, and was the main driver of differences in the nanoindentation deformation behaviour between these two types of silicon. Interestingly, in polycrystalline silicon, the HPPT was observed to occur more preferentially along the grain boundaries than across the grain boundaries. An automated dislocation extraction algorithm (DXA) revealed no dislocations in the deformation zone, suggesting that HPPT is the primary mechanism in inducing plasticity in silicon.

Indentation testing and its acoustic emission response: applications and emerging trends

Abstract This review summarises the state of knowledge on acoustic emission (AE) techniques applied to material property evaluation during indentation (e.g. hardness) testing. There are two aspects of application of AE technique to indentation which makes it unique, i.e. (1) enhancing the understanding of the evolution of material accommodation mechanisms under loading and (2) qualitative and quantitative evaluation of mechanical properties such as fracture toughness and bond strength from the AE signal. Both of these aspects have the potential to improve our understanding of the structure property relationships of current and future generation materials. In addition, the knowledge developed here can be incorporated to improve the AE based condition monitoring systems for stress critical applications. This review concentrates on the phenomena which occur during indentation and how its examination can be used to study more fundamental behaviour of materials such as deformation and fracture. The uncertainty in quantifying and measuring the total crack surface in indentation makes a simple fracture mechanics based assessment of toughness difficult. It is therefore expected that correlation between AE and fracture patterns will lead to an improved method for material’s quality evaluation. The main part of this review is presented on AE of material classifications. These classifications include ceramics, glasses, composites, metals and metallic foams, thin solid films and thermally sprayed coatings. Apart from quasi‐static indentation testing, attention has also been paid to studies on various AE instrumented indentation systems so that information can be derived about the progress of deformation and cracking processes. This review discusses the studies summarising those aspects that have so far been established and the areas of controversy and/or lack of knowledge. The prospect of using AE techniques to monitor indentation tests is also assessed, taking into account those few studies that have been reported so far in different groups of materials. Although with some limitations, it is concluded that AE monitored indentation testing has considerable scope to assess in much more detail the deformation and cracking properties of materials under localised stress condition. It is possible to construct empirical relationships and develop theoretical understanding linking mechanical parameters with AE signal characteristics and its derived features. However, the occurrence of multiple events at different locations superimposing the AE signal requires more advanced signal processing techniques. With the advancement of very thin films and nanomaterials, it is anticipated that AE response measured during nanoindentation will be critical for enhancing our understanding of future generation applications, as it allows individual events to be investigated without resorting to more complex signal processing techniques. In terms of material accommodation, the understanding of physical mechanisms generating AE require a multiscale approach, e.g. correlations exist between fracture and sudden release of AE energy, dislocations and Bremsstrahlung and Frank–Reid sources, and maternsitic phase transformation with rapid variation in the shape of deformation volume generating AE exist; however, integration of continuum elastic–plastic and molecular dynamics models is necessary to enhance our understanding of the physical mechanisms generating AE response. This multiscale approach can be further helped by the experimental data using AE instrumented nanoindentation as it allows very localised and fine scale measurement in load or displacement control.

Neutron diffraction residual strain measurements in nanostructured hydroxyapatite coatings for orthopaedic implants

The failure of an orthopaedic implant can be initiated by residual strain inherent to the hydroxyapatite coating (HAC). Knowledge of the through-thickness residual strain profile in the thermally sprayed hydroxyapatite coating/substrate system is therefore important in the development of a new generation of orthopaedic implants. As the coating microstructure is complex, non-destructive characterization of residual strain, e.g. using neutron diffraction, provides a useful measure of through thickness strain profile without altering the stress field. This first detailed study using a neutron diffraction technique, non-destructively evaluates the through thickness strain measurement in nanostructured hydroxyapatite plasma sprayed coatings on a titanium alloy substrate (as-sprayed, heat treated, and heat treated then soaked in simulated body fluid (SBF)). The influence of crystallographic plane orientation on the residual strain measurement is shown to indicate texturing in the coating. This texturing is expected to influence both the biological and fracture response of HA coatings. Results are discussed in terms of the influence of heat-treatment and SBF on the residual stress profile for these biomedical coatings. The results show that the through thickness residual strain in all three coatings was different for different crystallographic planes but was on average tensile. It is also concluded that the heat-treatment and simulated body fluid exposure had a significant effect on the residual strain profile in the top layers of HAC.

Structure Property Relationship of Suspension Thermally Sprayed WC-Co Nanocomposite Coatings

Tribomechanical properties of nanostructured coatings deposited by suspension high velocity oxy-fuel (S-HVOF) and conventional HVOF (Jet Kote) spraying were evaluated. Nanostructured S-HVOF coatings were obtained via ball milling of the agglomerated and sintered WC-12Co feedstock powder, which were deposited via an aqueous-based suspension using modified HVOF (TopGun) process. Microstructural evaluations of these hardmetal coatings included transmission electron microscopy, x-ray diffraction, and scanning electron microscopy equipped with energy dispersive x-ray spectroscopy. The nanohardness and modulus of the coated specimens were investigated using a diamond Berkovich nanoindenter. Sliding wear tests were conducted using a ball-on-flat test rig. Results indicated that low porosity coatings with nanostructured features were obtained. High carbon loss was observed, but coatings showed a high hardness up to 1000 HV2.9N. S-HVOF coatings also showed improved sliding wear and friction behavior, which were attributed to nanosized particles reducing ball wear in three-body abrasion and support of metal matrix due to uniform distribution of nanoparticles in the coating microstructure.

Influence of indenter shape on DLC film failure during multiple load cycle nanoindentation

Abstract The aim of the present investigation is to understand the localised failure mechanism of diamond-like carbon (DLC) film during multiple load cycle nanoindentation. The DLC film investigated was 500 nm thick sputter coated on Si (100) wafer of 500 μm thickness. Multiple load cycle nanoindentation tests under diamond Berkovich and conical indenters were performed using a calibrated NanoTest at five different load ranges between 0·1 and 500 mN. Test results indicated forward deviation, no deviation and backward deviation of the force–displacement profile, which provided some insights to the mechanisms of localised film failure. During backward deviation, film failure starts from interfacial delamination. This was observed for a conical indenter in a particular load range (1–10 mN). An elastic finite element model during nanoindentation loading indicated that this was caused by the location of maximum stress near the interface. Forward depth deviation was observed for conical and Berkovich indenter at all the other load ranges.

Fatigue at Nanoscale: An Integrated Stiffness and Depth Sensing Approach to Investigate the Mechanisms of Failure in Diamondlike Carbon Film

Nanoscale impact fatigue tests were conducted to comprehend the relative fatigue performance and failure modes of 100 nm thick diamondlike carbon (DLC) film deposited on a 4 in. diameter Si (100) wafer of 500 μm thickness. The nanofatigue tests were performed using a calibrated TriboIndenter equipped with Berkovich indenter in the load range of 300–1000 μN. Each test was conducted for a total of 999 fatigue cycles (a low cycle fatigue test). Contact depth in this load range varied from 10 to 30 nm. An integrated contact stiffness and depth sensing approach was adapted to understand the mechanisms of fatigue failure. The contact depth and stiffness data indicated some peculiar characteristics, which provided some insights into the mechanisms of cohesive and adhesive failure in thin films. Based on the contact stiffness and depth data, and surface observations of failed DLC films using atomic force microscope and scanning probe microscopy, a five-stage failure mechanism is proposed. The failure of films starts from cohesive failure via cracks perpendicular to the film/substrate interface, resulting in a decrease in contact depth with number of fatigue cycles and no appreciable change in contact stiffness. This is followed by film delamination at the film/substrate interface and release of elastic stored energy (residual stress) resulting in an increase in contact stiffness. Finally, as the film breaks apart the contact stiffness decreases with a corresponding increase in contact depth.

Neutron Diffraction Residual Strain Measurements in Plasma Sprayed Nanostructured Hydroxyapatite Coatings for Orthopaedic Implants

Residual strains in plasma sprayed and heat-treated hydroxyapatite (HA) coatings deposited on a titanium alloy (Ti-6Al-4V) substrate were investigated by means of neutron diffraction. Strain measurements were performed in vertical scan (“z-scanning”) mode to provide a through thickness strain profile in the coating and substrate materials. Results are discussed in terms of the influence of heat-treatment on the residual strain profile of these biomedical coatings. This investigation concluded that the heat-treatment had a significant effect on the residual strain profile in HA coatings.

An improved measurement of Vickers indentation behaviour through enhanced instrumentation

This work presents an enhanced instrumented Vickers indentation technique capable of recording force, displacement and acoustic emission (AE) during loading condition. Four materials were chosen for examination; copper, aluminium, steel and as-sprayed HVOF WC-12%Co coating. Results indicate that force–displacement (P–h) profiles are essentially bilinear with two characteristic slopes separated by a distinct displacement arrest for all loads above 98 N. The P–h curve indicates three distinct loading stages (I, II and III) and the stage III mechanical energy increases with loads. About 66% of the hardened steel indentations but only about 18% of the as-sprayed HVOF WC-12%Co coating indentations exhibited an AE record that could be separated into three distinct zones (A, B and C). Where zoning was possible the AE corresponding to a zone correlated well with the AE associated with a loading stage. It is concluded that plastic deformation in soft metals produced little AE, whereas brittle fracture in hardened steel and as-sprayed HVOF WC-12%Co coating produced significant AE. AE may or may not be focused onto particular stages of the indentation and a full measure of crack prevalence would require fractal dimension analysis, which is time consuming, offering a motivation for AE-based indentation testing.

Acoustic emission method to study fracture (Mode-I, II) and residual strength characteristics in composite-to-metal and metal-to-metal adhesively bonded joints

ABSTRACT Failure behaviour of two types of adhesively bonded joints (composite-to-metal, metal-to-metal) has been studied under failure modes (Mode I: double cantilever beam (DCB) and Mode II: three-point end notch flexures (3-ENF)) using acoustic emission (AE) technique. The bonded specimens were prepared using two types of adhesive bond materials with three variations of adhesive bond quality. The effect of the presence of interfacial defects along the interface on the residual strength of the joint has also been studied. It was possible using the maximum AE amplitude method to select the AE events of mechanical significance. However, it proved difficult to propose a definitive AE trait for the mechanical phenomena occurring within specific AE event signals, for all adhesive types, bond qualities, and substrate configurations, therefore, all specimen combinations. There was a notable shift in spectral energy proportion as the AE source of mechanical significance varied along the specimen length for specimen combinations. However, it was difficult to confirm this distinctive trait for all specimen combinations due to difficulty in confirming the location and exact mechanical source. The proposed measurement technique can be useful to assess the overall structural health of a bonded system and may allow identification of defects.

Influence of post-treatment on the microstructural and tribomechanical properties of suspension thermally sprayed WC-12 wt%Co nanocomposite coatings.

The potential to improve the tribomechanical performance of HVOF-sprayed WC–12Co coatings was studied by using aqueous WC–12Co suspensions as feedstock. Both as-sprayed and hot-isostatic-pressed (HIPed) coatings were studied. Mathematical models of wear rate based on the structure property relationships, even for the conventionally sprayed WC–Co hardmetal coatings, are at best based on the semiempirical approach. This paper aims to develop these semiempirical mathematical models for suspension sprayed nanocomposite coatings in as-sprayed and heat-treated (HIPed) conditions. Microstructural evaluations included transmission electron microscopy, X-ray diffraction and scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy. The nanohardness and modulus of the coated specimens were investigated using a diamond Berkovich nanoindenter. Sliding wear tests were conducted using a ball-on-flat test rig. Results indicated that the HIPing post-treatment resulted in crystallization of amorphous coating phases and increase in elastic modulus and hardness. Influence of these changes in the wear mechanisms and wear rate is discussed. Results are also compared with conventionally sprayed high-velocity oxy-fuel hardmetal WC–Co coatings.