Micromechanical Characterization of Electrophoretic-Deposited Green Films

Low-load indentation experiments have been performed on electrophoretic-deposited films of SiC particles on a graphite substrate. Films with thicknesses between 60 and 300 µm prepared at two current intensities and subsequently dried under different humidities were indented with spherical indenters with nominal radii of 10, 50, and 150 µm. Force-displacement data were analyzed to determine contact pressure and elastic modulus versus depth results. The modulus and contact pressure behavior with depth exhibited opposite trends with indenter radius: the modulus increase was least for the 10 µm and greatest for the 150 µm, whereas the contact pressure was the inverse. The results may be rationalized by plotting modulus normalized to the ratio "contact radius/film thickness" ( a / t ), whereas the contact pressure results at small a / t could be normalized when plotted versus contact strain, i.e., contact radius divided by indenter radius ( a / R ). These approaches enabled the properties of the variously deposited films to be compared. Additional interesting microstructural and cracking behavior patterns are also reported.     

Measurement of nanoindentation properties of polymers considering adhesion effects between AFM sharp indenter and material

Abstract

Nanomechanical properties of polymer samples were calculated using an adhesive contact model appropriate for AFM indentation problems. A series of Polydimethylsiloxane (PDMS) samples were indented by the sharp indenter in the air by using an AFM, and dozens of the force–displacement curves of each sample were obtained. An adhesive contact model suitable for sharp indentation with adhesion was established based on the same assumptions of the JKR model which is only suitable for spherical indentation at small penetration depth. Differences between sharp indentation problems with and without adhesion were discussed, and the limitations of the traditional adhesion model were given. The elastic modulus was obtained by fitting experimental force–displacement curves with theoretical ones, and results were compared to those macroscopic values in literature. The adhesion energy between the indenter and the sample surface was accurately calculated using the adhesion model based on the calculated elastic modulus. The influence of the indenter tip angle on the calculation results of the elastic modulus was also discussed theoretically. In this study, the mechanical properties of polymer samples were calculated at the nanoscale considering the adhesion effect.     

Characterization of oxidation film on SiC ceramic substrate based on indentation method

An indentation method is proposed to characterize the properties of oxidation film on a SiC ceramic substrate. In this method, a series of indentation tests on the oxidation film with different maximum indentation depths were performed. The relationship between the inverse of contact depth and the inverse of reduced modulus was fitted by an exponential function. The moduli of the oxidation film and substrate as well as the thickness of the oxidation film were estimated by analyzing the fitting parameters. In order to validate the method, indentation tests were conducted on SiC substrate to determine the reference modulus of the substrate. Microstructure observation was conducted to measure the reference thickness of the oxidation film. The estimated values agreed well with the reference values. Finite element analysis was also employed to simulate the indentation tests on the oxidation film. The simulation results agreed well with the experimental results.     

Nanoscale elastic-plastic deformation and stress distributions of the C plane of sapphire single crystal during nanoindentation

The nanoscale elastic-plastic characteristics of the C plane of sapphire single crystal were studied by ultra-low nanoindentation loads with a Berkovich indenter within the indentation depth less than 60 nm. The smaller the loading rate is, the greater the corresponding critical pop-in loads and the width of pop-in extension become. It is shown that hardness obviously exhibits the indentation size effect (ISE), which is 46.7 ± 15 GPa at the ISE region and is equal to 27.5 ± 2 GPa at the non-ISE region. The indentation modulus of the C plane decreases with increasing the indentation depth and equals 420.6 ± 20 GPa at the steady-state when the indentation depth exceeds 60 nm. Based on the Schmidt law, Hertzian contact theory and crystallography, the possibilities of activation of primary slip systems indented on the C surface and the distributions of critical resolved shear stresses on the slip plane were analyzed.     

Characterization of Films with Thickness Less than 10 nm by Sensitivity-Enhanced Atomic Force Acoustic Microscopy

We present a method for characterizing ultrathin films using sensitivity-enhanced atomic force acoustic microscopy, where a concentrated-mass cantilever having a flat tip was used as a sensitive oscillator. Evaluation was aimed at 6-nm-thick and 10-nm-thick diamond-like carbon (DLC) films deposited, using different methods, on a hard disk for the effective Young's modulus defined as E/(1 - ν ²), where E is the Young's modulus, and ν is the Poisson's ratio. The resonant frequency of the cantilever was affected not only by the film's elasticity but also by the substrate even at an indentation depth of about 0.6 nm. The substrate effect was removed by employing a theoretical formula on the indentation of a layered half-space, together with a hard disk without DLC coating. The moduli of the 6-nm-thick and 10-nm-thick DLC films were 392 and 345 GPa, respectively. The error analysis showed the standard deviation less than 5% in the moduli.     

Quantifying the mechanical properties of polymeric tubing and scaffold using atomic force microscopy and nanoindentation

Measurement of mechanical parameters of polymeric scaffolds presents a significant challenge due to their intricate shape and small characteristics dimensions of their elements—around 100 μm. In this study, mechanical properties of polymeric tubing and scaffold, made of biodegradable poly(l ‐lactic) acid (PLLA), were characterized using atomic force microscopy (AFM) and nanoindentation, complemented with tensile testing. AFM was employed to assess the properties of the tube and scaffold locally, while nanoindentation produced results with a dependency on the depth of indentation. As a result, the AFM‐measured elastic modulus differs from the nanoindentation data due to a substantial difference in indentation depth between the two methods. With AFM, a modulus between 2 and 2.5 GPa was measured, while a wide range was obtained from nanoindentation on both the tube and scaffold, depending on the indentation scale. Changes in the elastic modulus with in‐vitro degradation and aging were observed over the 1‐year period. To complement the indentation measurements, tensile testing was used to study the structural behavior of the tube, demonstrating the yielding, hardening and fracture properties of the material. POLYM. ENG. SCI., 59:1084–1091, 2019. © 2019 Society of Plastics Engineers     

An interaction stress analysis of nanoscale elastic asperity contacts

A new contact mechanics model is presented and experimentally examined at the nanoscale. The current work addresses the well-established field of contact mechanics, but at the nanoscale where interaction stresses seem to be effective. The new model combines the classic Hertz theory with the new interaction stress concept to provide the stress field in contact bodies with adhesion. Hence, it benefits from the simplicity of non-adhesive models, while offering the same applicability as more complicated models. In order to examine the model, a set of atomic force microscopy experiments were performed on substrates made from single-walled carbon nanotube buckypaper. The stress field in the substrate was obtained by superposition of the Hertzian stress field and the interaction stress field, and then compared to other contact models. Finally, the effect of indentation depth on the stress field was studied for the interaction model as well as for the Hertz, Derjaguin-Muller-Toporov, and Johnson-Kendall-Roberts models. Thus, the amount of error introduced by using the Hertz theory to model contacts with adhesion was found for different indentation depths. It was observed that in the absence of interaction stress data, the Hertz theory predictions led to smaller errors compared to other contact-with-adhesion models.     

Nanoindentation-induced delamination of submicron polymeric coatings

An elastic model is developed to estimate the interfacial strength between a submicron surface coating and a compliant substrate. The analysis uses a shear-lag model and assumes the plane-stress state in the surface coating. The critical indentation load for the indentation-induced delamination of the coating from the substrate increases with the third power of the indentation depth and is a linear function of the reciprocal of the coating thickness. The indentation-induced delamination of SR399 ultrathin surface coatings over acrylic substrate has been evaluated, using the nanonindentation technique for coating thicknesses of 47, 125, 220 and 3000 nm. For the submicron coatings, the dependence of the critical indentation load on the coating thickness supports the elastic model. The interfacial strength is found to be 46.9 MPa. In contrast, the polymeric coating of 3000 nm displays multiple “excursions” in the loading curve, and the critical indentation load is a linear function of the indentation depth.     

连续刚度法对单晶硅片的力学性能的表征

利用纳米压痕仪通过连续刚度测量法对单晶硅片在压入过程中的接触刚度、硬度、弹性模量进行了连续测量.结果表明:当接触深度在20～32 nm左右时,单晶硅片的接触刚度与接触深度成直线关系,硬度和弹性模量基本保持不变,此时所测得的是单晶硅片表面氧化层的硬度和弹性模量,分别约为10.2 GPa和140.3 GPa.当接触深度在32～60 nm左右时,单晶硅片的接触刚度与接触深度成非直线关系,硬度和弹性模量随接触深度急剧增加,表明单晶硅片表面氧化层的硬度和弹性模量受到了基体材料的影响.当接触深度在60 nm以上时,单晶硅片的接触刚度与接触深度成直线关系,硬度和弹性模量基本保持不变,测得值为单晶硅的硬度和弹性模量,分别约为12.5 GPa和165.6 GPa.     

Evaluation of the elastic-plastic properties of SiCN coating system by finite element simulations

The elastic properties of SiCN coating on substrates can be evaluated by nano-indentation test, however, it is challenging for experiments to evaluate the plastic performance of SiCN coating. Finite element (FE) is a numerical method for investigating in-depth mechanical behavior of various structures. In this paper, a contact model between Berkovich indenter and SiCN/Si system is established by FE method. The stress-strain behavior of SiCN coating is obtained by comparing the calculated P-h curves with experimental results. The indentation depth dependent elastic modulus and hardness of the SiCN coating are calculated from the P-h curves and are close to the experimental data. When the indentation depth is in excess of 10% of the coating thickness, the mechanical properties of SiCN coating tend to be influenced by the Si substrate, which also consists with experiments. The proposed approach provides an efficient tool to predict the mechanical properties of SiCN coating.     

Mechanical properties of porous methyl silsesquioxane and nanoclustering silica films using atomic force microscope

Mechanical properties of porous methyl silsesquioxane samples with dielectric constant 2.4 and 2.0 and a recently developed nanoclustering silica film samples with dielectric constants 2.3 and 2.0 were evaluated using an atomic force microscope based nanoindentation. It was found that the Young’s modulus and the hardness decrease while the fracture toughness increases with a decrease in the dielectric constant in the same type of material. Moreover, the Young’s modulus and the hardness of the nanoclustering silica films were observed to be at least twice and fracture toughness values ~1.3–1.5 higher than those for methyl silsesquioxane films with similar dielectric constants. The high resolution topographic imaging capability of atomic force microscope was shown to be particularly useful in the measurement of cracks generated by the ultra-low indentation loads, and the evaluation of the fracture toughness of the nanoscale volumes of materials.     

Indentation measurements using a dynamic mechanical analyzer

A dynamic mechanical analyzer equipped with a diamond indenter tip was used to measure the elastic modulus of polymeric coatings as well as various bulk materials. A fabricated indenter probe was used to indent bulk samples of aluminum and fused quartz, as well as gelatin and polystyrene films in order to compare the micron-level indentation measurements with sub-micron (nanoindentation) techniques. The measured moduli were in agreement for ductile materials and thick films (>20 μm), but limited displacement resolution, material cracking, and hydrostatic pressure effects led to diverging values for thinner coatings and more brittle materials.     

Determination of the elastic moduli of silicone rubber coatings and films using depth-sensing indentation

Depth-sensing indentation (DSI) has been used to determine the elastic moduli of silicone rubber coatings on substrates and freestanding films at micro-penetration depth. Complete elastic behavior for rubber-like films was observed for the first time. Substrate effects are hardly observed when the indentation displacement is less than 10% of the total coating thickness. The calculated elastic moduli of the silicone rubber films from the DSI measurements are in good agreement with those measured by dynamic mechanical analysis (DMA), showing that the DSI technique is a reliable and convenient tool for an accurate estimation of the elastic modulus of a rubber-like coating/film.     

Manufacture and characterization of free-standing epoxy-polyester films

The present investigation analyzes the deformation behaviour under static and dynamic loading conditions of electrostatically sprayed epoxy-polyester powder coatings by local and uniaxial tests, trying to account for the separate contribution of the raw polymeric material alone and of the adhesion to the underlying metal substrate. First, thermo-rheological properties of the basic material (i.e., the thermosetting powder paints) were characterized by differential scanning calorimetry (DSC) and rheometry. Secondly, free-standing films were manufactured by electrostatic spraying of the thermosetting powders onto stainless steel substrates pre-coated with an intermediate layer of silicon-based heat curable release coating. The resulting free standing-films were macroscopically characterized by combined dynamic-mechanical analyses (DMA) and tensile tests. Finally, local mechanical characterization of the coating performance was carried out by micro-scale depth sensing scratch and indentation on coatings ‘free-standing’ and ‘rigidly adhering’ onto metal substrate.     

Measurement approaches to develop a fundamental understanding of scratch and mar resistance

Instrumented indentation and confocal microscopy were used to characterize the surface mechanical response of polymeric materials. Viscoelastic behavior was measured using instrumented indentation. A model based on the contact between a rigid probe and a viscoelastic material was used to calculate values for the creep compliance and stress relaxation modulus for two polymeric materials, epoxy and poly(methyl methacrylate) or PMMA. Scratch testing was performed on these materials with various probes under a variety of conditions, and confocal microscopy was used to characterize the resulting deformation. Relationships among viscoelastic behavior, scratch damage, and appearance are currently being explored using these methods along with finite element modeling. Presented at the 81st Annual Meeting of the Federation of Societies for Coatings Technology, November 13–14, 2004, in Philadelphia, PA.     

Dynamic modulus of rubber by impact and rebound measurements

When rubber is deformed an energy input is involved which is released in part when the rubber returns to its original shape. The part which is not returned as mechanical energy is dissipated as heat. The “rebound resilience” is defined as the ratio of the energy returned to the energy applied for deformation by an indentation due to a single impact. In this experiment, a pendulum mass and a test piece, as long as they are in contact, may be considered an oscillating system having one degree of freedom in which the rubber is a Voigt model. The correlation between rebound resilience and loss angle of the rubber may thus be derived. The measurement of the contact time between pendulum indentor tip and rubber surface, in addition to the rebound resilience, allows calculation of deformation, speed and acceleration of the damped sinusoidal motion. The penetration of the spherical indentor under a constant force depends on Young's modulus. Scott found an empirical relationship among force applied, depth of indentation, radius of the indentor tip and the modulus. This relationship has been recently improved by Stiehler and coworkers, The Stiehler formula has been used here for evaluating the storage modulus of rubber vulcanizates by using the maximum force transmitted by the impacting mass and the indentation depth of the test piece at the same time.     

Viscoelasticity in Polymer Films on Rigid Substrates

The viscoelasticity of two thermally crosslinked polymer coatings was examined in terms of relaxation of the applied stress after a sudden strain. Two different transient methods were utilized: flat‐ended cylindrical indentation testing of a polymer film on a rigid substrate and tensile testing of a corresponding free‐standing polymer film. The correlation between tensile and indentation tests was studied. The mechanical response of a viscoelastic layer deposited on a rigid substrate was investigated as a function of indentation depth. There was good agreement between the results of the tensile and indentation tests for thick film layers at moderate indentation depths. The findings indicate that the substrate influences the coating performance by reducing the viscous contribution to the stress response and amplifying the magnitude of the equilibrium modulus for large indentation depths. The indentation method utilized here was shown to be a potentially suitable tool for the determination of Poisson's ratio of polymer films.

     

Mechanical characterization of polymeric films using depth-sensing instrument: Correlation between viscoelastic-plastic properties and scratch resistance

The scratch behavior of polymer films deposited on PMMA substrate by three different coating techniques is investigated by scratch tests using a depth-sensing instrument. Using an improved measurement technique, we develop an advanced methodology based on a more appropriated model that includes an estimation of realistic stress and strain states during scratch tests. The scratch resistance is evaluated by comparing the average contact pressure for which the coating cracks, by taking into account the elastic–plastic behavior of the layer. The proposed model allows the determination of the true contact depth and the elastic recovery at the rear side of the elastic–plastic contact, and thus the true projected contact area between the moving tip and the polymeric surface. This determination depends first on a rheological factor estimated from standard load–displacement curves obtained by nanoindentation and then on the tip geometry. The viscoplacticity index and the activation volume of each type of coating are then determined by nanoscratch. The viscoplasticity index determined during an elastic–plastic contact and the activation volume related to the ductile–brittle transition are discussed as reliable criteria for determining which bilayer system (polymeric film on PMMA substrate) will truly exhibit better wear and scratch resistances in service.     

Nanoindentation experiments for single-layer rectangular graphene films: a molecular dynamics study

A molecular dynamics study on nanoindentation experiments is carried out for some single-layer rectangular graphene films with four edges clamped. Typical load–displacement curves are obtained, and the effects of various factors including indenter radii, loading speeds, and aspect ratios of the graphene film on the simulation results are discussed. A formula describing the relationship between the load and indentation depth is obtained according to the molecular dynamics simulation results. Young’s modulus and the strength of the single-layer graphene film are measured as about 1.0 TPa and 200 GPa, respectively. It is found that the graphene film ruptured in the central point at a critical indentation depth. The deformation mechanisms and dislocation activities are discussed in detail during the loading-unloading-reloading process. It is observed from the simulation results that once the loading speed is larger than the critical loading speed, the maximum force exerted on the graphene film increases and the critical indentation depth decreases with the increase of the loading speed.     

Stepwise-Graded Si3N4–SiC Ceramics with Improved Wear Properties

The processing of stepwise graded Si₃N₄/SiC ceramics by pressureless co-sintering is described. Here, SiC (high elastic modulus, high thermal expansion coefficient) forms the substrate and Si₃N₄ (low elastic modulus, low thermal expansion coefficient) forms the top contact surface, with a stepwise gradient in composition existing between the two over a depth of ∼1.7 mm. The resulting Si₃N₄ contact surface is fine-grained and dense, and it contains only 2 vol% yttrium aluminum garnet (YAG) additive. This graded ceramic shows resistance to cone-crack formation under Hertzian indentation, which is attributed to a combined effect of the elastic-modulus gradient and the compressive thermal-expansion-mismatch residual stress present at the contact surface. The presence of the residual stress is corroborated and quantified using Vickers indentation tests. The graded ceramic also possesses wear properties that are significantly improved compared with dense, monolithic Si₃N₄ containing 2 vol% YAG additive. The improved wear resistance is attributed solely to the large compressive stress present at the contact surface. A modification of the simple wear model by Lawn and co-workers is used to rationalize the wear results. Results from this work clearly show that the introduction of surface compressive residual stresses can significantly improve the wear resistance of polycrystalline ceramics, which may have important implications for the design of contact-damage-resistant ceramics.