Molecular dynamic simulations of nanoindentation in aluminum thin film on silicon substrate

In the present work, the nanoindentation of aluminum thin film on silicon substrate is investigated by three-dimensional molecular dynamic (MD) simulation. The film/substrate system is modeled by taking Lennard-Jones (LJ) potential to describe the interaction at the film-substrate interface. Different loading rate from 50 to 250 m/s is carried out in the simulation. The results showed that the hardness of the film increased with the loading rate. In order to study the effect of substrate on the mechanical properties of thin film, nanoindentation process on monolithic Al material is also simulated. The simulation results revealed that indentation pile-up in the aluminum film is significantly enhanced by the substrate. The substrate also affects the loading force during the nanoindentation. At the beginning of the indentation, the loading force is not affected by the substrate. Then, it is getting smaller caused by the interface. As the film is penetrated, the loading force increased rapidly caused by the hard substrate. These results were coincident with the previous reported experiments.     

Analysis of the substrate effects of strain-hardening thin films on silicon under nanoindentation

Mechanical properties of thin films on substrates can be evaluated directly through nanoindentation. For a comprehensive study, thin films should be characterized via Young’s modulus, yield stress and strain-hardening exponent at constant temperature. In this paper, we evaluate these effects of thin films on silicon substrate through finite element analysis. Thin films, from soft to hard relative to the silicon substrate, are investigated in three categories: soft films on hard substrates, soft to hard films on no elastic mismatch substrates, and hard films on soft substrates. In addition to examining the load-displacement curve, the normalized hardness versus normalized indentation depth is checked as well to characterize its substrate effect. We found that the intrinsic film hardness can be acquired with indentation depths of less than 12% and 20% of their film thickness for soft films on hard substrates and for soft to hard films on no elastic mismatch substrates, respectively. Nevertheless, nanoindentation of hard films on soft substrates cannot determine the intrinsic film hardness due to the fact that a soft substrate cannot support a hard film. By examining the von Mises stresses, we discovered a significant bending phenomenon in the hard film on the soft substrate. PACS 61.43.Bn; 62.20.-x; 68.03.Hj; 68.05.Cf; 68.08.De     

Measurement of Residual Stresses Using Nanoindentation Method

Instrumented indentation, which is also known as nanoindentation or depth-sensing indentation, is increasingly being used to probe the residual stresses of materials including bulk solids, thin films, and coatings. The residual stresses are proved to have significant effects on various nanoindentation parameters such as hardness, loading curve, unloading curve, pile-up amount around indentation, and true contact area. By analyzing these parameters, numerous methods are developed to evaluate the residual stresses of materials in recent years. This article reviews six commonly used models which determine residual stresses from analyzing load-depth curves, as well as indentation fracture technique which is based on the classical fracture mechanics. Emphasis is placed on the principle, application and limitation of each nanoindentation method.     

Atomistic study of deposition process of Al thin film on Cu substrate

In this paper we report molecular dynamics based atomistic simulations of deposition process of Al atoms onto Cu substrate and following nanoindentation process on that nanostructured material. Effects of incident energy on the morphology of deposited thin film and mechanical property of this nanostructured material are emphasized. The results reveal that the morphology of growing film is layer-by-layer-like at incident energy of 0.1-10 eV. The epitaxy mode of film growth is observed at incident energy below 1 eV, but film-mixing mode commences when incident energy increase to 10 eV accompanying with increased disorder of film structure, which improves quality of deposited thin film. Following indentation studies indicate deposited thin films pose lower stiffness than single crystal Al due to considerable amount of defects existed in them, but Cu substrate is strengthened by the interface generated from lattice mismatch between deposited Al thin film and Cu substrate.     

Atomistic simulations of the effect of a void on nanoindentation response of nickel

Three-dimensional molecular dynamics simulations have been performed to investigate the effect of a void on the nanoindentation of nickel thin film.The radius and depth of the void are varied to explore how they influence the nanoindentation.The simulation results reveal that the presence of a void softens the material and allows for a larger indentation depth at a given load compared to the no void case.The radius and depth of the void have a major effect on the indentation behaviors of the thin film.It is also observed that the void will collapse during the nanoindentation of crystal with void.And when the indentation depth is sufficiently large,the void will disappear.It is found that the indentation depth needed to make the void disappear depends on the void size and location.     

Fracture force analysis at the interface of Pd and SrTiO3

The objective of this work is to develop an experimental indentation based method to determine the fracture force at the interface of Pd thin films and SrTiO₃ perovskite substrate. This paper reports on the results obtained for indentation into Pd thin films which were deposited in various thicknesses from 20 nm to 200 nm under vacuum and 300 °C substrate temperature by an electron beam physical vapor deposition. Initially, the relation between grain size, elastic module and hardness was considered as a function of film thickness. Thereafter, in developing new method, oscillating indentation was performed with different applied forces and oscillating times in order to measure the critical fracture force in each thickness. The effect of oscillating time on plastically deformed regions surrounding an indentation was schematically explained in conjunction with variation of oscillating time to determine the interfacial properties of the Pd thin film. Furthermore, the accuracy of the critical fracture force was ensured by applied force versus piling up height plot. The method is validated experimentally for the soft thin films over the hard substrate. However, further study would be essential to measure the film adhesion by means of fracture force at the interface.     

Mechanical properties of sol-gel derived lead zirconate titanate thin films by nanoindentation

Lead zirconate titanate (PZT) thin films are deposited on platinized silicon substrate by sol-gel process. The crystal structure and surface morphology of PZT thin films are characterized by X-ray diffraction and atomic force microscopy. Depth-sensing nanoindentation system is used to measure mechanical characteristics of PZT thin films. X-ray diffraction analyses confirm the single-phase perovskite structures of all PZT thin films. Nanoindentation measurements reveal that the indentation modulus and hardness of PZT thin films are related with the grain size and crystalline orientation. The increases of the indentation modulus and hardness with grain size are observed, indicating the reverse Hall-Petch effect. Furthermore, the indentation modulus of (1 1 1)-oriented PZT thin film is higher than those of (1 0 0)- and random-oriented films. The consistency between experimental data and numerical results of the effective indentation moduli for fiber-textured PZT thin films using Voigt-Reuss-Hill model is obtained.     

Nanomechanical characteristics of SnO2:F thin films deposited by chemical vapor deposition

The nanoindentation characterizations and mechanical properties of fluorine-doped tin oxide (SnO₂:F) films deposited on glass substrates, using chemical vapor deposition (CVD) method, were studied, which included the effects of the indentation loads, the loading time and the hold time on the thin film. The surface roughness, fractal dimension and frictional coefficient were also studied by varying the freon flow rates. X-ray diffraction (XRD), atomic force microscopy (AFM) and frictional force microscopy (FFM) were used to analyze the morphology of the microstructure. The results showed that crystalline structure of the film had a high intensity (1 1 0) peak orientation, especially at a low freon flow rate. According to the nanoindentation records, the Young's modulus ranged from 62.4 to 75.1 GPa and the hardness ranged from 5.1 to 9.9 GPa at a freon flow rate of 8000 sccm. The changes in measured properties were due to changing loading rate.     

Dynamic characteristics of nanoindentation in Ni:A molecular dynamics simulation study

In this work,three-dimensional molecular dynamics simulation is carried out to elucidate the nanoindentation behaviour of single crystal Ni.The substrate indenter system is modelled using hybrid interatomic potentials including the manybody potential(embedded atom method) and two-body Morse potential.The spherical indenter is chosen,and the simulation is performed for different loading rates from 10 m/s to 200 m/s.Results show that the maximum indentation load and hardness of the system increase with the increase of velocity.The effect of indenter size on the nanoindentation response is also analysed.It is found that the maximum indentation load is higher for the large indenter whereas the hardness is higher for the smaller indenter.Dynamic nanoindentation is carried out to investigate the behaviour of Ni substrate to multiple loading-unloading cycles.It is observed from the results that the increase in the number of loading unloading cycles reduces the maximum load and hardness of the Ni substrate.This is attributed to the decrease in recovery force due to defects and dislocations produced after each indentation cycle.     

Theoretical study on nanoindentation hardness measurement of a particle embedded in a matrix

The finite element method was used to simulate indentation tests on a particle embedded in a matrix, to investigate the influence of the properties of the particle and the matrix, and the indentation depth on the measured hardness. The particle’s work-hardening exponent and the mismatch in particle and matrix yield strength have a significant influence on the measured hardness. A particle-dominated indentation depth was identified, within which the measured nanoindentation hardness agrees very well with the true hardness of the particle material. Numerical results from the simulations of a wide range of material properties determined that the measured hardness is within 5% difference of the particle’s true hardness when the indentation depth is less than 13.5% of the particle’s radius. The results can be used in practice as a guideline to measure the hardness of a particle embedded in a matrix and provides the theoretical basis to develop a particle-embedded method to measure the hardness of individual particles.     

Nanoindentation Experimental Approach and Numerical Simulation of Al/Cr Bilayer Films

The Al/Cr double-layer film structure samples (thickness, 1200 nm) were prepared by the magnetron sputtering method. To investigate the mechanical properties, the samples were measured by using a nanoindentation instrument. The test results showed the nonlinearity and different modes of the main mechanical properties by comparing the macro-scale structure samples with other samples of similar materials. Based on the test, the elastic modulus and hardness of thin film structures can be calculated by considering different loads to conduct multi-point indentations. Meanwhile, the relationships between the mechanical parameters can be investigated based on these Al/Cr double-layer film structure samples. To validate the test, numerical analysis was developed using a finite element method to simulate the loading and unloading process of indentation. The simulation results were compared with the results of experiments to illustrate the validity of both the test and simulation to a certain extent. The investigation builds not only an experimental basis for practical applications for future study, but also supplies a complementary means of verification for theoretical analysis.     

Mechanical and tribological properties of Ni/Al multilayers—A molecular dynamics study

Mechanical and tribological properties of multilayers with nanometer thickness are strongly affected by interfaces formed due to mismatch of lattice parameters. In this study, molecular dynamics (MD) simulations of nanoindentation and following nanoscratching processes are performed to investigate the mechanical and tribological properties of Ni/Al multilayers with semi-coherent interface. The results show that the indentation hardness of Ni/Al multilayers is larger than pure Ni thin film, and the significant strength of Ni/Al multilayers is caused by the semi-coherent interface which acts as a barrier to glide of dislocations during nanoindentation process. The confinement of plastic deformation by the interface during nanoscratching on Ni/Al multilayers leads to smaller friction coefficient than pure Ni thin film. Dislocation evolution, interaction between gliding dislocations and interface, variations of indentation hardness and friction coefficient are studied.     

Nanoindentation study of size effect and loading rate effect on mechanical properties of a thin film metallic glass Cu49.3Zr50.7

A binary metallic glass (MG) Cu_49.3Zr_50.7 in the form of thin film was successfully grown on a Si (1 0 0) substrate by magnetron sputtering. The mechanical properties, specifically, hardness and modulus at various peak loads and loading rates were characterized through instrumented nanoindentation. Unlike other metallic glasses showing an indentation size effect (ISE), the composition of this study does not have an ISE, which is phenomenologically the result of the negligible length scale according to the strain gradient plasticity model. The proportional specimen resistance model is applicable to the load-displacement behaviors and suggests that the frictional effect is too small to contribute to the ISE. The occurrence of plasticity depends on loading rates and can be delayed so that the displacement during the load holding segment increases logarithmically. In addition, the hardness and modulus are both dependent on the loading rates as well, i.e., they increase as the loading rate increases up to 0.1 mN/s and then hold constant, which is independent of creep time (≤100 s). These loading-rate-dependent behaviors are interpreted as the result of viscoelastic effect rather than free volume kinetics.     

Investigation of material properties of thin copper films through finite element modelling of microindentation test

Technology processes of thin metal films deposition are entailed with changes in material’s microstructure. As a result, deposited films often are characterized with material properties, which are different from these of the original bulk material. Determination of these material characteristics is of big importance for practice. In the present work the material properties of thin bright copper film with known depth were investigated. The film was deposited electrochemically over substratum composed of metallurgic brass alloy (CuZn36). Based on the results from microindentation test the load-displacement curve is obtained after the indenter is unloaded and the imprint diameter is measured. Consequently the process of indentation was modelled numerically. The numerical simulation is based on the finite element model of the indentation process. As a result of the simulation the load-displacement curve was obtained numerically for a certain set of material parameters. The trial-error approach is applied to find most appropriate set which fit the experimental load-displacement curve. At the end results, which were obtained through numerical simulation give good coincidence with the experiment. Therefore the proposed method can be successfully applied for identification of material parameters of the accepted model. The proposed trial-error approach is appropriate for investigation of thin films with known thickness, deposited on a substrate with known material characteristics.     

Identifying the viscoelastic properties of soft matter from the indentation response of a hard film-soft substrate system

The indentation technique is widely used in measuring the mechanical properties of soft matter at the microscale or nanoscale,but still faces challenges by these unique properties as well as the consequent strong surface adhesion, including the strong nonlinear effect, unclear judgment of the contact point, difficulties in estimating the contact area, and the risk of the indenter piercing the sample. Here we propose a two-step method to solve these problems: lay a hard film on a soft matter, and obtain the viscoelastic properties of this soft matter through the indentation response of this composite structure. We first establish a theoretical indentation model of the hard film-soft substrate system based on the theory of plates, elastic-viscoelastic correspondence principle and Boltzmann superposition principle. To verify the correctness of this method, we measure the mechanical properties of the methyl vinyl silicone rubber(MVSR) covered by a Cu nanofilm. Finally, we test the effectiveness and error sensitivity of this method with the finite element method(FEM). The results show that our method can accurately measure the mechanical properties of soft matter, while effectively circumventing the problems of the traditional indentation technique.     

Effect of substrate curvature on thickness distribution of polydimethylsiloxane thin film in spin coating process

The polymer spin coating is critical in flexible electronic manufaction and micro-electro-mechanical system(MEMS)devices due to its simple operation, and uniformly coated layers. Some researchers focus on the effects of spin coating parameters such as wafer rotating speed, the viscosity of the coating liquid and solvent evaporation on final film thickness.In this work, the influence of substrate curvature on film thickness distribution is considered. A new parameter which represents the edge bead effect ratio(re) is proposed to investigate the influence factor of edge bead effect. Several operation parameters including the curvature of the substrate and the wafer-spin speed are taken into account to study the effects on the film thickness uniformity and edge-bead ratio. The morphologies and film thickness values of the spin-coated PDMS films under various substrate curvatures and coating speeds are measured with laser confocal microscopy. According to the results, both the convex and concave substrate will help to reduce the edge-bead effect significantly and thin film with better surface morphology can be obtained at high spin speed. Additionally, the relationship between the edge-bead ratio and the thin film thickness is like parabolic curve instead of linear dependence. This work may contribute to the mass production of flexible electronic devices.     

Reverse analysis in depth-sensing indentation for evaluation of the Young's modulus of thin films

This paper presents an approach to reverse analysis in depth-sensing indentation of composite film/substrate materials, which makes use of numerical simulation. This methodology allows the results of experimental hardness tests, acquired with pyramidal indenter geometry, to be used to determine the Young's modulus of thin film materials. Forward and reverse analyses were performing using three-dimensional numerical simulations of pyramidal and flat punch indentation tests to determine the Young's modulus of the thin films. The pyramidal indenter used in the numerical simulations takes into account the presence of the most common imperfection of the tip, so-called offset. The contact friction between the Vickers indenter and the deformable body is also considered. The forward analysis uses fictitious composite materials with different relationships between the values of the Young's modulus of the film and substrate. The proposed reverse analysis procedure provides a unique value for the film's Young's modulus. Depending on material properties, the value of the Young's modulus of the film can be more or less sensitive to the scatter of the experimental results obtained using the depth-sensing equipment. The validity of the proposed reverse analysis method is checked using four real cases of composite materials.     

Simulation of the interface characterization of thin film on substrate system by bending creep tests

In the present paper, the finite element simulation of the bending creep tests of the thin film on substrate system is carried out. The purpose of the investigation is to understand the creep stress characterization of the thin film on substrate system with the three points bending creep test method, which plays an important role in the bending creep testing characterization, so as to provide some foundation on determination of interface properties of the thin film on substrate system by a bending creep testing. Finite element results shows that the influences of the thickness of thin film and the modulus ratio of thin film to substrate on stress distribution are important.     

Finite-element analysis of the mechanical behavior of Au/Cu and Cu/Au multilayers on silicon substrate under nanoindentation

Finite-element analysis of the nanoindentation into Au/Cu and Cu/Au multilayers was performed to deduce their mechanical characteristics from nanoindentation response. Different bilayer thicknesses, numbers, and sequences were studied using the load–displacement curve, hardness, indentation, and the residual surface profile as well as the von Mises equivalent stress. The characteristics of the multilayers were found to be dispersed between the Au and Cu. Nevertheless, if the indentation depth is smaller than the uppermost individual layer thickness of the multilayers, the intrinsic properties can be obtained. Using the von Mises equivalent stress as a failure criterion, the results showed that thinner multilayers would induce a greater potential of shear banding deformation. PACS 61.43.Bn; 62.20.-x; 68.03.Hj; 68.05.Cf; 68.08.De     

Effect of substrate interactions on the melting behavior of thin polyethylene films

Polymer films have been known to change their physical properties when film thickness is decreased below a certain value. The cause of this phenomenon is still unclear but it has been suggested that interactions and/or chain free-volume changes at the surface of the films are largely responsible for this behavior. In this paper, the effect of substrate interactions on the behavior of polymer thin films is evaluated quantitatively. The infrared spectra of nanothin polyethylene (PE) films were recorded as a function of temperature and amount of substrate covering the surface of the film. The evolution of specific bands in the CH₂ rocking region of the spectra was used to determine the melting temperature (T _m ) of the material. Results show different variations in T _m depending on the nature of the substrate, indicating that interactions dominate free-volume considerations in PE thin films. By varying the amount of surface coverage, a quantitative estimate of the heat of interaction was determined, which confirmed the importance of surface interactions.