Indentation Load Effect on Young＇s Modulus and Hardness of Porous Sialon Ceramic by Depth Sensing Indentation Tests

Depth sensing indentation （DSI） tests at the range of 200-1800mN are performed on porous sialon ceramic to determine the indentation load on Young＇s modulus and hardness values. The Young modulus and hardness （Dynamic and Martens） values are deduced by analysing the unloading segments of the DSI test load-displacement curves using the Oliver-Pharr method. It is found that Young＇s modulus ET, the dynamic hardness HD and the Martens hardness HM exhibit significant indentation load dependences. The values of Young＇s modulus and hardness decrease with the increasing indentation load, as a result of indentation load effect. The experimental hf /hm ratios lower than the critical value 0.7, with hm being the maximum penetration depth during loading and hf the final unloading depth, indicate that our sample shows the work hardening behaviour.     

Elastic–plastic deformation of Pb(Zn1/3Nb2/3)O3–(6–7)% PbTiO3 single crystals during nanoindentation

The elastic–plastic deformation behavior of (001)- and (011)-oriented single crystal solid solutions of Pb(Zn_1/3Nb_2/3)O₃–(6–7)% PbTiO₃ (PZN–PT) have been studied using a nanoindentation technique. A procedure is presented here to isolate the elastic, elastic–plastic and plastic contributions to the deformation using the unloading data, and a parameter, referred to as relaxation, is defined to characterize the elastic–plastic deformation during nanoindentations. This relaxation parameter increases with the maximum indentation load due to the higher indentation stress induced, and it also causes less recovery of the material upon indentation unloading compared to predicted pure elastic recovery. For a (001) surface, the relaxation value remains virtually unchanged within the range of the maximum indentation load of 10–50 mN, possibly due to a complete localized depoling of the non-180° domain switching. It is also found that the unpoled surface is more prone to stress-induced depolarization compared to the poled surfaces. Furthermore, by applying the continuous stiffness measurement (CSM) technique, the effects of multiple loading/unloading are studied for both (001)- and (011)-oriented PZN–PTs using the maximum indentation loads of 20 and 50 mN. With more loading/unloading cycles at higher CSM frequencies, stress-induced depolarization becomes prevalent and the contribution of the domain reorientation towards elastic recovery is significantly reduced. As a consequence, the relaxation value is increased, indicating more elastic–plastic deformation. This CSM effect is especially pronounced for poled (011) surfaces.     

Nanoindentation measurements on modified diamond-like carbon thin films

In the present study, we explored the effect of metallic interlayers (Cu and Ti) and indentation loads (5-20 mN) on the mechanical properties of plasma produced diamond-like carbon (DLC) thin films. Also a comparison has been made for mechanical properties of these films with pure DLC and nitrogen incorporated DLC films. Introduction of N in DLC led to a drastic decrease in residual stress (S) from 1.8 to 0.7 GPa, but with expenses of hardness (H) and other mechanical properties. In contrast, addition of Cu and Ti interlayers between substrate Si and DLC, results in significant decrease in S with little enhancement of hardness and other mechanical properties. Among various DLC films, maximum hardness 30.8 GPa is observed in Ti-DLC film. Besides hardness and elastic modulus, various other mechanical parameters have also been estimated using load versus displacement curves.     

Dynamic ball hardness tests on polymers

The present work demonstrates the possibility of determining and differentiating the elastic and plastic material properties (like the Young's modulus, the ball hardness under load, and the plastic hardness) by applying the dynamic ball hardness indentation test. In Ref. 1, the elastic properties are neglected. Nevertheless, the obtained hardness number includes both elastic and plastic parts. Now, the continuous data acquisition allows the determination of the elastic modulus of the polymer and also its dynamic and thermal dependence. Furthermore, a way of specifying a plastic hardness number is shown. Using the approach of Oliver and Pharr [2] enables the separation of the real material property of plastic hardness. Topographic measurements allowed taking the wall formation during a hardness test into account while analyzing the impression. It turned out that the elastic modulus determined in the manner described is independent of the penetration rate, but decreases with increasing temperature or caoutchouc mass content. Also, the dynamic and thermal dependence of the hardness are discussed.     

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.     

Study of water uptake in poly(ether ether ketone) irradiated by MeV O+ and Au+ ions

Poly(ether ether ketone) (PEEK) was irradiated with 4?MeV O⁺ and 5 and 10?MeV Au⁺ ions to the fluences from 10¹² to 10^14?cm^?2 and then treated in 5 M/l water solution of LiCl for one month at room temperature. After drying and removal of LiCl surface contamination, the depth distribution of LiCl embeded in PEEK was measured by the neutron depth profilig method (NDP) sensitive to ⁶Li isotope. Embeded LiCl is believed to map distribution of water diffusing into PEEK interior. The results show that the PEEK irradiated to the fluences above 1.10¹³cm^?2 is prone to water penetration to the depths of few microns. On the pristine PEEK and that irradiated to lower ion fluences only a surface Li contamination is observed.     

Gamma radiation effects on mechanical properties and morphology of a polyurethane derivate from castor oil

In this study, an adhesive of a polyurethane derivate from castor oil was irradiated with gamma radiation from a ⁶⁰Co source, at doses from 0.2 to 25 kGy. This adhesive polyurethane is considered for use in hospital furniture because it does not liberate dangerous solvents. Hardness and elastic modulus were measured by instrumented indentation with a pyramidal Berkovich indenter, using loads from 0.08–40 mN with a nanoindenter XP. The instrumented indentation hardness was 110 MPa for an untreated sample, increasing to 124 MPa after irradiation with 25 kGy, at penetration depths of about 5 μm. The increases in elastic modulus induced by radiation were less pronounced. This polyurethane is naturally cross-linked and the relative modifications in the hardness are attributed to an additional cross-linking process induced by radiation. X-ray diffraction indicates a slight increase in crystallinity. The roughness measured by atomic force microscopy increases after gamma irradiation.     

Identification of elastic-plastic and phase transition characteristics for relaxor ferroelectric PMN-PT anisotropic single crystals using nanoindentation technique

As one kind of important ferroelectric ceramics, relaxor ferroelectric PMN-PT single crystals have triggered a revolution in electromechanical devices owing to their giant piezoelectric properties and ultra-high electromechanical coupling factors. The present study focused on the mechanical responses of [100]- and [110]-oriented poled PMN-PT ferroelectric single crystals under an indenter loading. The hardness and Young’s modulus with different crystallographic orientations of the crystals were measured by using the continuous stiffness measurement (CSM) with nanoindentation technique. Using a spherical indenter pressured at different indentation depths, the typical quasi-static nanoindentation tests with displacement-controlled mode were performed on the PMN-PT single crystal samples. Load–displacement curves of indentations were recorded to reveal the yielding or inelasticity behaviour in [100]- and [110]-oriented PMN-PT through a pop-in event. It was further verified by the stress–strain curves evaluated from the corresponding load–displacement curves, to show the similar characteristic on the elastic–inelastic transition. When a Berkovich indenter was employed for mechanical response testing, another pop-in event was observed at a smaller indentation depth compared to the one for elastic–inelastic transition, which may indicate a pressure-induced phase transition from rhombohedral (R) to tetragonal (T) of the PMN-PT single crystals.     

光学元件亚表层裂纹成核临界条件研究

基于压痕实验和连续刚度测量法得到了熔石英材料硬度和弹性模量随压入深度的变化曲线, 系统分析了材料由延性到脆性转变的过程, 确定了熔石英晶体在静态/准静态印压和动态刻划时产生裂纹的临界载荷和临界深度。渐变载荷刻划实验结果表明, 划痕过程诱发的裂纹对法向载荷有很强的依赖性, 载荷较小时材料去除方式为延性域去除。随着法向载荷的增加, 首先产生垂直于试件表面的中位裂纹和平行于试件表面方向扩展的侧向裂纹, 而在试件表面上并没有产生明显的特征。载荷进一步增加后, 侧向裂纹扩展并形成了明亮区域, 最终诱发了沿垂直于或近似垂直于压头运动方向扩展的径向裂纹, 实现了材料的脆性去除。     

Effect of chemical etching on the Cu/Ni metallization of poly (ether ether ketone)/carbon fiber composites

Poly(ether ether ketone)/carbon fiber composites (PEEK/Cf) were chemical etched by Cr₂O₃/H₂SO₄ solution, electroless plated with copper and then electroplated with nickel. The effects of chemical etching time and temperature on the adhesive strength between PEEK/Cf and Cu/Ni layers were studied by thermal shock method. The electrical resistance of some samples was measured. X-ray photoelectron spectroscopy (XPS) was used to analyze the surface composition and functional groups. Scanning electron microscopy (SEM) was performed to observe the surface morphology of the composite, the chemical etched sample, the plated sample and the peeled metal layer. The results indicated that CO bond increased after chemical etching. With the increasing of etching temperature and time, more and more cracks and partially exposed carbon fibers appeared at the surface of PEEK/Cf composites, and the adhesive strength increased consequently. When the composites were etched at 60 °C for 25 min and at 70-80 °C for more than 15 min, the Cu/Ni metallization layer could withstand four thermal shock cycles without bubbling, and the electrical resistivity of the metal layer of these samples increased with the increasing of etching temperature and time.