A method to determine fracture toughness using cube-corner indentation

For the cube-corner indenter, an approximate linear relationship between the ratio of hardness (H) to reduced modulus (E-r) and the ratio of unloading work (W-u) to total loading work (W-t) is confirmed by finite-element calculations and by experiments. Based on this relationship a convenient method to determine the fracture toughness (K-IC) of brittle materials, especially for those at small scale, using cube-corner indentations is proposed. Finally, the method is calibrated by indentation experiments on a set of brittle materials. (C) 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

电磁式纳米压入仪的载荷精度研究

纳米压入仪(Nanoindenter)已成为纳米/微米力学测试的基本工具之一,广泛应用于纳米材料、薄膜、MEMS微结构的力学性能测试。目前商业化仪器有MTS NanoIndenter(incorporated into Agi lent in 2008),Hysitron TriboIndenter,CSM NanoHardness Tester,MML NanoTest,and CSIRO UMIS,其中原MTS Nano Indenter、CSMNano Hardness Tester和MML NanoTest都采用电磁驱动兼载荷计量的原理设计。这类仪器主要优点之一是载荷分辨力高,可以达到50nN甚至更小。然而仪器制造商从未明确给出此类仪器的载荷精度。目前对纳米压痕测试技术的研究也主要集中在压头形状、试样表面粗糙度、毛细力等因素对压痕测试结果的影响,尚未见针对仪器载荷精度的研究报道。国际标准ISO 14577-2:2002虽对仪器施加的试验力的允差进行了规定,但由于电磁式纳米压入仪的结构响应和试样力学行为耦合在一起,试样上的载荷并不完全等同于通过电磁转换原理计量的试验力,因此实际测试时试样上的载荷精度仍是未知。

纳米压痕仪的载荷精度研究

<正>以MTS Nano Indenter(?)XP为例,研究发现了影响电磁式纳米压痕仪载荷精度的两个重要因素。其一,磁场的均匀性。在实验位移范围内磁场必须是均匀的,这是电磁计量载荷的理论基础。校准实验结果显示,NanoIndenter(?)XP在0.45mm位移行程内的非均匀性为0.24%。即,在0.45mm位移行程内磁场均匀性给载荷

Mechanical Behavior of Nanometer Ni by MD Simulation

The indention simulation of the crystal Ni is carried out by molecular dynamics technique (MD) to study the mechanical behavior at nanometer scales, the indenter tips with sphere shape is used. Some defects such as dislocations, point defects are observed. It is found that defects (dislocations, amorphous) nucleated is from local region near the pin tip or the sample surface. The temperature distribution of local region is analyzed and it can explain our MD simulation result.

Indentation of power law creep solids by self-similar indenters

For creep solids obeying the power law under tension proposed by Tabor, namely sigma = b(epsilon) over dot(m), it has been established through dimensional analysis that for self-similar indenters the load F versus indentation depth h can be expressed as F(t) = bh(2)(t)[(h) over dot(t)/h(t)](m)Pi(alpha) where the dimensionless factor Pi(alpha) depends on material parameters such as m and the indenter geometry. In this article, we show that by generalizing the Tabor power law to the general three dimensional case on the basis of isotropy, this factor can be calculated so that indentation test can be used to determine the material parameters b and m appearing in the original power law. Hence indentation test can replace tension test. This could be a distinct advantage for materials that come in the form of thin films, coatings or otherwise available only in small amounts. To facilitate application values of this constant are given in tabulated form for a range of material parameters. (C) 2010 Elsevier B.V. All rights reserved.

Influence of Contact Geometry on Hardness Behavior in Nano-indentation

In this paper the influence of contact geometry, including the round tip of the indenter and the roughness of the specimen, on hardness behavior for elastic plastic materials is studied by means of finite element simulation. We idealize the actual indenter by an equivalent rigid conic indenter fitted smoothly with a spherical tip and examine the interaction of this indenter with both a flat surface and a rough surface. In the latter case the rough surface is represented by either a single spherical asperity or a dent (cavity). Indented solids include elastic perfectly plastic materials and strain hardening elastic-plastic materials, and the effects of the yield stress and strain hardening index are explored. Our results show that due to the finite curvature of the indenter tip the hardness versus indentation depth curve rises or drops (depending on the material properties of the indented solids) as the indentation depth decreases, in qualitative agreement with experimental results. Surface asperities and dents of curvature comparable to that of the indenter tip can appreciably modify the hardness value at small indentation depth. Their effects would appear as random variation in hardness.

Synthesis and properties of a novel isomeric polyimide/SiO2 hybrid material

A novel isomeric polyimide/SiO2 hybrid material was successfully prepared through sol-gel technique, and its structure, thermal properties and nano-indenter properties were investigated. First, 3-[(4-phenylethynyl)phthalimide]propyl triethoxysilane (PEIPTES) was successfully synthesized, its structure was characterized by elemental analysis, FT-IR and C-13 NMR. The researches on solubility and thermal properties of PEIPTES show that it can be used for modifying nano-SiO2 precursor. Nano-SiO2 precursor was synthesized by tetraethoxysilane (TECS) through sol-gel technique. Then the PEIPTES solution and the nano-SiO2 precursor were mixed for 6 h to let the PEIPTES molecules react with the nano-SiO2 precursor, and modified nano-SiO2 precursor was obtained. The modified reaction was confirmed by the analyses of FT-IR. At last, isomeric polyimide/SiO2 hybrid material was produced by using isomeric polyimide resin solution and the modified nano-SiO2 precursor after heat treatment process. The structure analysis by SEM indicated that SiO2 particles dispersed in isomeric polyimide matrix homogeneously with nanoscale. Thermogravimetric analyzer, dynamic mechanical thermal analyzer and nano-indenter XP was employed to detect the properties of the materials, the results demonstrated that isomeric polyimide/SiO2 hybrid material has much better thermal properties and nano-indenter properties than those of isomeric polyimide.

Hardness of covalent crystals

Based on the idea that the hardness of covalent crystal is intrinsic and equivalent to the sum of the resistance to the indenter of each bond per unit area, a semiempirical method for the evaluation of hardness of multicomponent crystals is presented. Applied to beta-BC2N crystal, the predicted value of hardness is in good agreement with the experimental value. It is found that bond density or electronic density, bond length, and degree of covalent bonding are three determinative factors for the hardness of a polar covalent crystal. Our method offers the advantage of applicability to a broad class of materials and initializes a link between macroscopic property and electronic structure from first principles calculation.

藏东南迦巴瓦变质岩楔入体东边界阿尼桥断裂带构造变形性质、年代学与构造意义

The Namche Barwa metamorphic rock indenter is a part of the Indian plate. The Aniqiao fault, a northeastern striking shear zone, is the eastern boundary of the Namche Barwa metamorphic rock indenter. The activities of the Aniqiao fualt reflects the history of structure deformation and uplift of the Namche Barwa metamorphic rock indenter. In this dissertation, studied the history of activities of the Aniqiao fault, I study the deformation of the Namche Barwa metamorphic rock indenter based on which, I try to discuss the history of action and deformation of the eastern Tibet. The Aniqiao fault composes of mica quartz schist. With observing in the field and by the microscope, there are at least two stages of deformation. The earlier is right lateral striking, the later is normal striking. The biotite, in the hornblende biotitic mylonite in western footwall, the muscovite and sericite, in the mica quartz schist in eastern hangingwall, show 4 plateau and isochron ages: 3.7-3.3Ma, 6.8-6.4Ma, 13.4-13.2Ma, 23.9Ma, by ~(40)Ar/~(39)Ar. Combine the characteristics of kinematics with the characteristics of isotopic ages, this dissertation figured three stages of deformation: in 23.9Ma and 13.4-13.2 Ma, the Aniqiao fault undertook twice strike-slip deformation; in 6.8Ma-6.4Ma, the Aniqiao fault occurred normal strike deformation; in 3.7-3.3Ma, there was another thermal case which maybe relating to uplift. Combine the deformation of the Aniqiao fault and the deformation of the western boundary fault of the Namche Barwa metamorphic rock indenter, this dissertation considers that the Namche Barwa metamorphic rock indenter has occurred three defomational cases during the period of Oligocene and Quaternary: in 23Ma and 13Ma, the Namche Barwa metamorphic rock indenter wedged into the Gangdisi granite zone; from 6-7Ma, the Namche Barwa metamorphic rock indenter begins to uplift. From 6-7Ma, the Namche Barwa metamorphic rock indenter must has been occurred multi-stage uplifting. The indentation of the Namche Barwa metamorphic rock indenter is correspond to the structure escape of the Chuanxi, Dianxi blocks. In the surface deformation, the movement of these blocks are very harmonious.

Silica polymer bonding of stressed silica grains: An early growth of intergranular tensile strength

© 2015 Elsevier Ltd. All rights reserved.Laboratory tests on microscale are reported in which millimeter-sized amorphous silica cubes were kept highly compressed in a liquid environment of de-ionized water solutions with different silica ion concentrations for up to four weeks. Such an arrangement simulates an early evolution of bonds between two sand grains stressed in situ. In-house designed Grain Indenter-Puller apparatus allowed measuring strength of such contacts after 3-4 weeks. Observations reported for the first time confirm a long-existing hypothesis that a stressed contact with microcracks generates silica polymers, forming a bonding structure between the grains on a timescale in the order of a few weeks. Such structure exhibits intergranular tensile force at failure of 1-1.5 mN when aged in solutions containing silica ion concentrations of 200-to 500-ppm. The magnitude of such intergranular force is 2-3 times greater than that of water capillary force between the same grains.

X-ray diffraction, optical microscopy, and microhardness studies of gas nitrided titanium alloys and titanium aluminide

Thermochemical surface gas nitriding of ß21s, Timetal 205 and a Ti–Al alloy was conducted using differential scanning calorimeter equipment, in nominally pure nitrogen at 850 °C and 950 °C (ß21s), 730 °C and 830 °C (Timetal 205), and 950 °C and 1050 °C (Ti–Al) for 1 h, 3 h and 5 h. X-ray diffraction analyses showed new phases formed in the nitrided layer, depending on the alloy and the time and the temperature of nitriding. Microstructures were analyzed using optical microscopy. Cross-sectional microhardness profiles of cross-sectional samples after nitriding were obtained using a Knoop indenter.

Experimental and numerical studies on rock breaking with TBM tools under high stress confinement

The understanding of rock breaking and chipping due to the TBM cutter disks mechanism in deep tunnels is considered in this paper. The interest stems from the use of TBMs for the excavation of long Trans-Alpine tunnels. Some tests that simulate the disk cutter action at the tunnel face by means of an indenter, acting on a rock specimen are proposed. The rock specimen is confined through a flat-jack and a confinement-free area on one side of the specimen simulates the formation of a groove near the indenter, like it occurs in TBM excavation conditions. Results show a limited influence of the confinement stress versus the thrust increment required for breaking the rock between the indenter and the free side of the specimen. Numerical modelling of the cutter disk action on confined material has also been carried out in order to investigate further aspects of the fracture initiation. Also in this case the importance of the relative position between disk cutter and groove is pointed out. © 2006 Springer-Verlag.

Laboratory tests to study the influence of rock stress confinement on the performances of TBM discs in tunnels

To clarify some aspects of rock destruction with a disc acting on a high confined tunnel face, a series of tests were carried out to examine fracture mechanisms under an indenter that simulates the tunnel boring machine (TBM) tool action, in the presence of an adjacent groove, when a state of stress (lateral confinement) is imposed on a rock sample. These tests proved the importance of carefully establishing the optimal distance of grooves produced by discs acting on a confined surface, and the value (as a mere order of magnitude) of the increase of the thrust to produce the initiation of chip formation, as long as the confinement pressure becomes greater. © University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg 2011.

Incipient plasticity in 4H-SiC during quasistatic nanoindentation

Silicon carbide (SiC) is an important orthopaedic material due to its inert nature and superior mechanical and tribological properties. Some of the potential applications of silicon carbide include coating for stents to enhance hemocompatibility, coating for prosthetic-bearing surfaces and uncemented joint prosthetics. This study is the first to explore nanomechanical response of single crystal 4H-SiC through quasistatic nanoindentation. Displacement controlled quasistatic nanoindentation experiments were performed on single crystal 4H-SiC specimen using a blunt Berkovich indenter (300 nm tip radius) at extremely fine indentation depths of 5 nm, 10 nm, 12 nm, 20 nm, 25 nm and 50 nm. Load-displacement curve obtained from the indentation experiments showed yielding or incipient plasticity in 4H-SiC typically at a shear stress of about 21 GPa (~an indentation depth of 33.8 nm) through a pop-in event. An interesting observation was that the residual depth of indent showed three distinct patterns: (i) Positive depth hysteresis above 33 nm, (ii) no depth hysteresis at 12 nm, and (iii) negative depth hysteresis below 12 nm. This contrasting depth hysteresis phenomenon is hypothesized to originate due to the existence of compressive residual stresses (upto 143 MPa) induced in the specimen by the polishing process prior to the nanoindentation

Influence of test methodology and probe geometry on nanoscale fatigue mechanisms of diamond-like carbon thin film

The aim of this paper is to investigate the mechanism of nanoscale fatigue using nano-impact and multiple-loading cycle nanoindentation tests, and compare it to previously reported findings of nanoscale fatigue using integrated stiffness and depth sensing approach. Two different film loading mechanism, loading history and indenter shapes are compared to comprehend the influence of test methodology on the nanoscale fatigue failure mechanisms of DLC film. An amorphous 100 nm thick DLC film was deposited on a 500 μm silicon substrate using sputtering of graphite target in pure argon atmosphere. Nano-impact and multiple-load cycle indentations were performed in the load range of 100 μN to 1000 μN and 0.1 mN to 100 mN, respectively. Both test types were conducted using conical and Berkovich indenters. Results indicate that for the case of conical indenter, the combination of nano-impact and multiple-loading cycle nanoindentation tests provide information on the life and failure mechanism of DLC film, which is comparable to the previously reported findings using the integrated stiffness and depth sensing approach. However, the comparison of results is sensitive to the applied load, loading mechanism, test-type and probe geometry. The loading mechanism and load history is therefore critical which also leads to two different definitions of film failure. The choice of exact test methodology, load and probe geometry should therefore be dictated by the in-service tribological conditions, and where necessary both test methodologies can be used to provide better insights of failure mechanism. Molecular dynamics (MD) simulations of the elastic response of nanoindentation is reported, which indicates that the elastic modulus of the film measured using MD simulation was higher than that experimentally measured. This difference is attributed to the factors related to the presence of material defects, crystal structure, residual stress, indenter geometry and loading/unloading rate differences between the MD and experimental results.