Mechanical properties of porous silicon by depth-sensing nanoindentation techniques

Porous silicon (PS) was prepared using the electrochemical corrosion method. Thermal oxidation of the as-prepared PS samples was performed at different temperatures for tuning their mechanical properties. The mechanical properties of as-prepared and oxidized PS were thoroughly investigated by depth-sensing nanoindentation techniques with the continuous stiffness measurements option. The morphology of as-prepared and oxidized PS was characterized by field emission scanning electron microscope and the effect of observed microstructure changes on the mechanical properties was discussed. It is shown that the hardness and Young's elastic modulus of as-prepared PS exhibit a strong dependence on the preparing conditions and decrease with increasing current density. In particular, the mechanical properties of oxidized PS are improved greatly compared with that of as-prepared ones and increase with increasing thermal oxidation temperature. The mechanism responsible for the mechanical property enhancement is possibly the formation of SiO₂ cladding layers encapsulating on the inner surface of the incompact sponge PS to decrease the porosity and strengthen the interconnected microstructure.     

Study of the mechanical properties of CeO2 layers with the nanoindentation technique

The mechanical properties of CeO₂ layers that are undoped or doped with other elements (e.g. Zr and Ta) are a topic of special interest specially in the manufacturing of superconductor buffer layers by pulsed electron deposition. Nowadays, the trend is to produce small devices (i.e. coated conductors), and the correct mechanical characterization is critical. In this sense, nanoindentation is a powerful technique widely employed to determine the mechanical properties of small volumes. In this study, the nanoindentation technique allow us determine the hardness (H) and Young's modulus (E) by sharp indentation of different buffer layers to explore the deposition process of CeO₂ that is undoped or doped with Zr and Ta, and deposited on Ni–5%W at room temperature. This study was carried out on various samples at different ranges of applied loads (from 0.5 to 500 mN). Scanning electron microscopy images show no cracking for CeO₂ doped with Zr, as the doping agent increases the toughness fracture of the CeO₂ layer. This system, presents better mechanical stability than the other studied systems. Thus, the H for Zr–CeO₂ is around 2.75 · 10⁶ Pa, and the elastic modulus calculated using the Bec et al. and Rar et al. models equals 249 · 10⁶ Pa and 235 · 10⁶ Pa respectively.     

Size effect of indenter on determining modulus of nanowires using nanoindentation technique

This study uses a finite element modeling to simulate the behavior of copper nanowires submitted to nanoindentation and estimate their mechanical properties. The simulation results reveal that using the well-known Oliver-Pharr theory, generally applied for materials with semi-infinite half-space, yields an underestimate elastic modulus of the wire materials. Moreover, the radius of the indenter tip also influences the accuracy of the predicted elastic modulus. Such errors are mainly from the overestimate of the contact area between the indenter and the specimen. They can be corrected from the numerical modeling. The elastic modulus of the wires calculated from the corrected contact area is highly close to the bulk value.     

Localized elastic modulus distribution of nanoclay/epoxy composites by using nanoindentation

The enhancement of mechanical properties by the use of nanoclay platelets in epoxy resin has been extensively investigated through numerous experimental techniques recently. Elastic modulus was obtained mainly from the tensile test of bone-like nanoclay/epoxy specimens. The results from the tensile test have only showed the globalized mechanical properties of composites and their localized elastic modulus distribution has been neglected. Despite the orientation and the degree of exfoliation of nanoclay platelets inside nanoclay/epoxy composites, the localized elastic modulus is important for the understanding of the distribution of agglomerations of nanoclay platelets. The elastic modulus of nanoclay/epoxy composite samples made under different sonication temperatures would be examined by nanoindentation to compare their localized mechanical behaviors. Scanning electron microscopy (SEM) would also be employed to study the distribution of the nanoclay clusters throughout the composites. The results showed that the elastic modulus varied throughout the composites and the nucleation theory of clusters was modified to explain the behavior of nanoclay agglomerations under different sonication temperatures in which the viscosity of the epoxy resin was varied. The gravitational effect was significant to cause the non-uniform distributions of nanoclay clusters at low sonication temperature.     

A simple sol-gel technique for synthesis of nanostructured hydroxyapatite, tricalcium phosphate and biphasic powders

Hydroxyapatite (HAP), β-tricalcium phosphate (β-TCP) and biphasic calcium phosphate (BCP) nanocrystalline powders were prepared by a simple sol-gel approach. Because of the unique characteristic of the phosphorous source ((CH₃O)₃P) and the proper uses of calcic and phosphorous sources with Ca/P molar ratio between 1.4 and 1.67, three different kinds of nanostructured calcium phosphate powders were achieved by changing the ratio of calcic and phosphorous sources. For HAP and β-TCP, pure phases were prepared. For BCP, the proportion of HAP and β-TCP could be changed by thermal treatment.     

Mechanical properties of single crystal tungsten microwhiskers characterized by nanoindentation

The nanoindentation results in this work showed that the one-dimensional single crystal tungsten microwhiskers fabricated by vapor deposition possess unique yielding behavior. The average hardness of the microwhiskers measured on their (1 1 1) surfaces was 8.44 GPa, significantly higher than that of the bulk tungsten ranged from 3.4 to 5.8 GPa. The hardness increase was attributed to the lacking of dislocation avalanche in the 1D single crystal tungsten that was often observed in the nanoindentation of the bulk tungsten. However, the values of elastic modulus of the microwhiskers measured on the (1 1 1) surfaces were considerably scattered, whose average value is much lower than the reported value of 410 GPa for the bulk tungsten.     

Representative indentation elastic modulus evaluated by unloading of nanoindentation made with a point sharp indenter

The conventional method to extract elastic modulus from the nanoindentation on isotropic linearly elastic solids is based on Sneddon’s solution (1965). However, it is known that the solution is valid only for incompressive elastic solids with the Poisson’s ratio ν of 0.5. This paper first proposes the modification of the solution in a wide range of ν from 0 to 0.5 through the numerical analysis on the unloading behavior of a simulated conical nanoindentation with a finite element method. As a result of the modification, the coefficient of linearity between the indentation elastic parameter k_e and Young’s modulus E is empirically given as a function of ν and the inclined face angle of the indenter, β, where k_e is defined as k_e ≡ P/h² with the indentation load P and penetration depth of the indenter h. According to the linear relationship between k_e and E, it is found that elastic rebound during unloading of a nanoindentation is uniquely characterized by a representative indentation elastic modulus E¹ defined in terms of E, ν and β, and that the value of E¹ can be evaluated from the P–h relationship with k_e and β. For an isotropic elastoplastic solid, the indentation unloading parameter k₂ defined as k₂ ≡ P/(h–h_r)² for a residual depth h_r is different from k_e even though a linearly elastic solid with k_e and elastoplastic solid with k₂ have a common E¹. In order to evaluate E¹ of an elastoplastic solid, the corresponding k_e is estimated from k₂ with an empirical equation as a function of the relative residual depth ξ defined as ξ ≡ h_r/h_max for the maximum penetration depth h_max. A nanoindentation experiment confirmed the validity of the numerical analysis for evaluating the elastic modulus.     

Nanoindentation mapping of mechanical properties of cement paste and natural rocks

This paper reports a study to assess nanoindentation mapping of mechanical properties of cement paste and natural rocks. Initial work seems to show that mechanical property mapping by nanoindentation is feasible and can be related to microscopic information. Further work is however required on the effect of indent size and spacing. Such a testing technique can be very useful for materials with different phases to study the intrinsic properties of each component, and also the interaction and properties of the interfacial regions of different phases. The values of Young's modulus and hardness of the individual mineral phases were also determined by statistically analysing a large number of experimental data.     

Creep Behavior and Its Influence on the Mechanics of Electrodeposited Nickel Films

In order to improve the accuracy and comparability of hardness and elastic modulus measurements in nanoin-dentation, an evaluation of the creep behavior and its influence on the mechanical properties of the electrode-posited nickel film has been conducted. The influence of loading time and hold period on the hardness and elastic modulus results at maximum load 5000 μN has also been examined. It is found that with increasing the loading time, the creep value is decreased. However, the creep value is increased when the hold period is increased. The elastic modulus results are more reliable if the hold period is longer. If the hold period is long enough, the loading time has no remarkable effect on the hardness and elastic modulus measured.     

Measuring mechanical properties of plasma-sprayed alumina coatings by nanoindentation technique

AISI 1020 steel substrate is coated with alumina as feedstock material using plasma spraying process in order to correlate the microstructural features with mechanical properties of coating. The present work focuses on the effects of microstructural inhomogeneity on mechanical properties of alumina coating through nanoindentation technique. Young’s modulus and hardness of the alumina coating are analytically evaluated. Indentation stress–strain curves are generated from the experimentally obtained load–displacement curves to characterise the mechanical properties of the coating. The results have shown large variation in hardness and Young’s modulus of alumina due to microstructural inhomogeneity of the coating.     

纳米压痕仪和激光超声技术检测薄膜弹性模量

在薄膜材料的力学性能测定中,弹性模量是衡量材料软硬程度的重要指标。为了测定弹性模量,本文选取不同种类和厚度的金属薄膜材料,采用纳米压痕技术(nanoindentation)和激光超声技术(laser-acoustics)两种测试方法相互比较,以确保测试的准确性。两种方法在膜厚较大的试样测试中得到了大致相符的试验结果,相对误差最小达到2%。     

Inkjet printing of conductive Ag lines and their electrical and mechanical characterization

This paper aims to investigate the effects of the substrate, the printed line thickness and the sintering temperature on the electrical resistivity, Young's modulus and hardness of inkjet-printed Ag thin films. Electrical resistivity was determined from the four-point method and Young's modulus and hardness were evaluated from nanoindentation test. Several models for evaluating Young's modulus and hardness were used and compared to account for the influence of substrates. It is noted that Ag lines on glass have higher resistance and resistivity than those on polyimide (PI) since Ag lines on glass and PI have tensile and compressive residual thermal stresses, respectively, due to the difference of coefficient of thermal expansion between Ag lines and substrates. Young's modulus of Ag films on glass can be predicted by the modified King and Bec models considering the substrate effect, but these models offer unstable results for Ag films on PI. Young's modulus and hardness of Ag films increase with the sintering temperature, and they are little affected by the film thickness when fully sintered.     

Application of causality check and of the reduced variables method for experimental determination of Young''s modulus of a viscoelastic material

An accurate determination of the complex dynamic Young's modulus of a viscoelastic material, in a broad frequency range, is presented in this paper. Curves of Young's modulus of the tested material (a mixture of polypropylene and calcium carbonate), at different temperatures, are experimentally obtained by means of a laser sensor. The experimental curves are then gathered into a unique master curve, by applying the reduced variables method and a causality check on the curves. The master curve represents Young's modulus of the viscoelastic material over a much broader frequency range, with respect to the range of a single experimental curve.     

Effect of metal-ion-to-fuel ratio on the phase formation of bioceramic phosphates synthesized by self-propagating combustion

Synthetic calcium hydroxyapatite (HAP, Ca₁₀ (PO₄)₆ (OH)₂) is a well-known bioceramic material used in orthopedic and dental applications because of its excellent biocompatibility and bone-bonding ability due to its structural and compositional similarity to human bone. Here we report, for the first time, the synthesis of HAP by combustion employing tartaric acid as a fuel. Calcium nitrate is used as the source of calcium and diammonium hydrogen phosphate serves as the source of phosphate ions. Reaction processing parameters such as the pH, fuel-oxidant ratio and autoignition temperature are controlled and monitored. The products were characterized by powder x-ray diffraction, which revealed the formation of a hexagonal hydroxyapatite phase. Fourier transform infrared spectroscopy (FT-IR) spectra showed that the substitution of a carbonate ion occurs at the phosphate site. The morphology of the particles was imaged by scanning electron microscopy, which also revealed that the particles are of submicron size. Thermal analysis showed that the phase formation takes place at the time of combustion. Surface area and porosity analysis showed that the surface area is high and that the pores are of nanometer size. The mean grain size of the HAP powder, determined by the Debye–Scherrer formula, is in the range 20–30 nm. Chemical analyses to determine the Ca : P atomic ratio in synthesized ceramics were performed, and it was found to be 1 : 1.66.     

Effect of metal-ion-to-fuel ratio on the phase formation of bioceramic phosphates synthesized by self-propagating combustion

Abstract

Synthetic calcium hydroxyapatite (HAP, Ca₁₀ (PO₄)₆ (OH)₂) is a well-known bioceramic material used in orthopedic and dental applications because of its excellent biocompatibility and bone-bonding ability due to its structural and compositional similarity to human bone. Here we report, for the first time, the synthesis of HAP by combustion employing tartaric acid as a fuel. Calcium nitrate is used as the source of calcium and diammonium hydrogen phosphate serves as the source of phosphate ions. Reaction processing parameters such as the pH, fuel-oxidant ratio and autoignition temperature are controlled and monitored. The products were characterized by powder x-ray diffraction, which revealed the formation of a hexagonal hydroxyapatite phase. Fourier transform infrared spectroscopy (FT-IR) spectra showed that the substitution of a carbonate ion occurs at the phosphate site. The morphology of the particles was imaged by scanning electron microscopy, which also revealed that the particles are of submicron size. Thermal analysis showed that the phase formation takes place at the time of combustion. Surface area and porosity analysis showed that the surface area is high and that the pores are of nanometer size. The mean grain size of the HAP powder, determined by the Debye–Scherrer formula, is in the range 20–30 nm. Chemical analyses to determine the Ca : P atomic ratio in synthesized ceramics were performed, and it was found to be 1 : 1.66.     

Effect of carbon on the density,microstructure and hardness of alloys formed by mechanical alloying

This work aimed to produce iron-based alloys containing resistant microstructures to improve the mechanical properties of the resulting alloy. The effects of both carbon content and compaction pressure on the microstructure, density and hardness of the alloys were examined. Iron-based alloys with initial carbon contents of 0.5%, 1%, 2% and 3% were produced by powder metallurgy following a process that involved ball milling elemental powders, cold pressing and sintering. The composition, density, microstructure, porosity, hardness and ductility of the alloys depended on both compaction pressure and carbon content. As the carbon content increased, the amount of the resistant microstructure bainite in the alloys also increased, as did their hardness. In contrast, the density and ductility of the alloys decreased with increasing carbon content. This study shows that formation of the resistant microstructure bainite in alloys fabricated by powder metallurgy is influenced by both the initial carbon content of the alloy and compaction pressure during cold pressing.     

Mechanical properties determined by nanoindentation tests of [Pb(Zr,Ti)O3] and [Pb(Mg1/3Nb2/3)1−xTixO3] sputtered thin films

As the introduction of piezoelectric materials into micro electromechanical systems increases, there is a correlating requirement for understanding the mechanical properties of these films. We have investigated the mechanical properties of unpoled PZT [Pb(Zr,Ti)O₃] and PMNT [Pb(Mg_1/3Nb_2/3)_1−xTi_xO₃] thin films deposited by sputtering. In this study, nano-indentation, a technique which allows determination of the transverse mechanical properties, is used. It is the easiest method for assessing the biaxial elastic modulus and the hardness of thin films. It was confirmed that neither cracks, nor pile-ups, were observed for indentation depths below 20% of the film's thickness.The continuous stiffness method was used and allowed us to demonstrate that the indentation modulus decreases continuously with increasing grain diameter. This can be explained by the orientation changes of the crystallites with increasing grain diameter. The indentation modulus measured under load, or at almost null load (that is when the ferroelectric domains are or are not oriented by the stress) are coherent with those determined by the same method with a hard bulk ceramic. These results tend to show that the compliance C_ij of the hard bulk ceramic can possibly be used with sputtered thin films. The hardness is almost independent of the grain diameter (H_b ≅ 7.5 ± 0.9 GPa) and higher than that for the bulk PZT ceramics considered in this study. PMNT and PZT films have appreciably the same mechanical characteristics. No influence of the film thickness was found on the values of both of these parameters.     

Surface effects on Young’s modulus and hardness of fused silica by nanoindentation study

The surface Young’s modulus (E) and hardness (H) of fused silica samples have been studied by nanoindentation. Two factors strongly affect the results of E and H. One factor is the polishing quality of the fused silica surface. Poor polishing quality produces much smaller E and H than the literature values for bulk fused silica. The second factor is surface flatness. Even for a well-polished silica surface, an “arch bridge effect” may hinder the measurements of the true values of E and H. A correction procedure is proposed to eliminate this effect, and the corrected results show substantial improvements.     

Determination of mechanical properties of thermally grown oxide on Fecralloy by nano-indentation

Nano-indentation was used to measure the mechanical properties of the thermally grown oxide (TGO) on a Fecralloy substrate. Due to the influence both of the substrate and the indenter size effect (ISE), the measured hardness and Young's modulus of the TGO system decreased with increasing indentation depth. Models were proposed to determine the mechanical properties of the TGO with consideration of both the substrate effect and the ISE. In addition, the ratio of hardness to Young's modulus (H/E) can be related to the ratio of irreversible work to total work (W_ir/W_t) during the indentation process.     

Surface morphology,elastic modulus and hardness of thin film cathodes for Li-ion rechargeable batteries

In this study, surface morphology, elastic modulus and hardness of two thin film cathode materials, namely layered structured LiNi_1/3Co_1/3Mn_1/3O₂ and spinel structured LiMn₂O₄, during the charge/discharge cycles, are measured by using Scanning Electron Microscopy, Atomic Force Microscopy and nanoindentation experiments. Furthermore, the effects of depth of discharge (DOD) and charging rate (current density) on the changes of elastic modulus and hardness of the spinel structured LiMn₂O₄ are also investigated. The results have shown that both elastic modulus and hardness of the thin film cathodes have been significantly affected by the charge/discharge cycles as well as the condition of the charge/discharge processes. These results suggest the importance of the mechanical properties of the cathode materials to the reliability and integrity of the cathode materials to be used for the Li-ion batteries. The possible mechanisms of the changes in mechanical properties are also discussed.