Identification of stiffness tensor components of wood cell walls by means of nanoindentation

A new procedure to characterize the full set of elastic constants of wood cell walls was developed. For the first time, not only the longitudinal modulus, but also the transverse- and the shear modulus were determined in one experimental setup at micron scale. For this purpose, nanoindentation experiments were performed at variable angles between the indentation direction and the direction of cellulose microfibrils in wood cell walls. Using an approach based on anisotropic indentation theory a relationship between the indentation moduli obtained experimentally and the elastic material constants of the cell wall was derived. Using an error minimization procedure, the values of the elastic material constants were finally calculated. As typically observed for natural materials, our experimental results are characterized by high variability. Particularly the elastic modulus in longitudinal cell direction is highly sensitive to small changes in the local orientation of cellulose microfibrils. Nonetheless, reasonable estimates of 26.3 GPa for the longitudinal elastic modulus of the secondary wood cell wall S2, 4.5 GPa for the transverse modulus, and – for the first time – a value of 4.8 GPa for the shear modulus of wood cell wall material were obtained.     

Direct measurements of interfacial shear strength of multi-walled carbon nanotube/PEEK composite using a nano-pullout method

This paper presents a proposal of a simple and easy method to evaluate the interfacial shear strength (IFSS) of CNT-dispersed polymer composites. An individual multi-wall carbon nanotube (MWNT) was pulled out from a MWNT-dispersed/PEEK composite using a nano-pullout testing system installed in an SEM. The tensile load was measured using the elastic deformation of an AFM cantilever. The pull-out length was controlled by making a through-thickness hole near the specimen edge using a focused ion beam (FIB) system. The IFSS of a MWNT/PEEK composite was measured as 3.5-14 MPa, which agrees with the IFSS estimated from the macroscopic stress-strain behavior of the MWNT/PEEK composites.     

Design and characterization of nanoknife with buffering beam for in situ single-cell cutting

A novel nanoknife with a buffering beam is proposed for single-cell cutting. The nanoknife was fabricated from a commercial atomic force microscopy (AFM) cantilever by focused-ion-beam (FIB) etching technique. The material identification of the nanoknife was determined using the energy dispersion spectrometry (EDS) method. It demonstrated that the gallium ion pollution of the nanoknife can be ignored during the etching processes. The buffering beam was used to measure the cutting force based on its deformation. The spring constant of the beam was calibrated based on a referenced cantilever by using a nanomanipulation approach. The tip of the nanoknife was designed with a small edge angle 5° to reduce the compression to the cell during the cutting procedure. For comparison, two other nanoknives with different edge angles, i.e. 25° and 45°, were also prepared. An in situ single-cell cutting experiment was performed using these three nanoknives inside an environmental scanning electron microscope (ESEM). The cutting force and the sample slice angle for each nanoknife were evaluated. It showed the compression to the cell can be reduced when using the nanoknife with a small edge angle 5°. Consequently, the nanoknife was capable for in situ single-cell cutting tasks.     

Visual force sensing with flexible nanowire buckling springs

A calibrated method of force sensing is demonstrated in which the buckled shape of a long flexible metallic nanowire, referred to as a 'nanoneedle', is interpreted to determine the applied force. An individual needle of 157?nm diameter by 15.6?μm length is grown on an atomic force microscope (AFM) cantilever with a desired orientation (by the method of Yazdanpanah et al 2005 J. Appl. Phys. 98 073510). Using a nanomanipulator the needle is buckled in the chamber of a scanning electron microscope (SEM) and the buckled shapes are recorded in SEM images. Force is determined as a function of deflection for an assumed elastic modulus by fitting the shapes using the generalized elastica model (De Bona and Zelenika 1997 Proc. Inst. Mech. Eng. C 211 509-17). In this calibration the elastic modulus (68.3?GPa) was determined using an auxiliary AFM measurement, with the needle in the same orientation as in the SEM. Following this calibration the needle was used as a sensor in a different orientation than the AFM coordinates to deflect a suspended PLLA polymer fiber from which the elastic modulus (2.96?GPa) was determined. The practical value of the sensing method does depend on the reliability and ruggedness of the needle. In this study the same needle remained rigidly secured to the AFM cantilever throughout the entire SEM/AFM calibration procedure and the characterization of the nanofiber.     

Determination of the flexural strength and elastic modulus of ice from in situ cantilever-beam tests

From the theory of cantilever beams on an elastic foundation, it is shown that the strength index and modulus index of ice can be determined from measurements of either the failure load or the tip deflection, or both, of in situ cantilever beams tested over a wide enough range of ratio of beam length to beam thickness. Four methods are proposed, two of which do not require the measurement of beam deflection during beam loading, an often difficult task to perform with sufficient reliability, especially in the field. The methods have been applied to available field and laboratory data. The initial results show reasonably consistent estimates of the strength index but a large variation in the predicted values of the modulus index. One preferred method is suggested but its validity and reliability need to be further evaluated by analyzing a sufficient number of field and laboratory tests.     

On the influence of residual stress on nano-mechanical characterization of thin coatings

In the present paper, the effect of residual stress on the mechanical behavior of thin hard coatings has been investigated by a new methodology based on the combined use of focused ion beam (FIB) micro-machining techniques and nanoindentation testing. Surface elastic residual stress were determined by nanoindentation testing on Focused Ion Beam (FIB) milled micro-pillars. The average residual stress present in a 3.8 microm CAE-PVD TiN coating on WC-Co substrate was calculated by the comparison of two different sets of load-depth curves, the first one obtained at centre of stress relieved pillars, the second one on the undisturbed (residually stressed) surface. Results for stress measurement were in good agreement with the estimate obtained by XRD (sin2 psi method) analysis on the same sample, adopting the same elastic constants. In addition, nanoindentation on stress relieved pillars also allowed to perform a more accurate evaluation of elastic modulus and hardness of the coating. The effect of residual stress on crack propagation modes was quantitatively analyzed by high-load nanoindentation and application of energy methods for fracture toughness evaluation. It is found that compressive residual stress plays a relevant role in determining the fracture behavior and failure modes of the coating. Finally, Microstructural observations of the deformation mechanisms of the TiN coating were performed by TEM analysis on the cross section of the indentation, obtained by FIB lamella thinning. Results showed that plastic deformation at the nanoscale essentially occurs by formation of shear bands inside the columnar grains, independently of residual stress. A transition between intra-granular shear deformation and columnar grain sliding is also observed as a function of the applied load.     

Cell wall properties and their effects on the mechanical properties of fibers

The properties of the cell wall are determined by its structure and by the properties of the wood polymers. In this study, the influence of the elastic constants of the three wood polymers on the elastic modulus of the cell wall was investigated. Cellulose was found to dominate the properties in the longitudinal direction. In the transverse direction, the effect of the properties of hemicellulose was more pronounced. The results show that it is possible to reduce the discrepancy between experimental and modeled values of the transverse modulus to a large extent by lowering the assumed values of the elastic constants of hemicellulose and lignin. The thickness and fibril angles of the S₁- and S₃-layers were also found to be important parameters for the transverse properties of the fiber wall. These two layers should not be neglected when transverse elastic properties are related to cell wall structure.     

Effects of low temperature on the dynamic moduli of thick composite beams with absorbed moisture

The present investigation concentrates on the influence of low temperature and moisture on the dynamic moduli of thick S2-glass composite beams. By supporting the beam sample in a free–free configuration, its natural frequencies were obtained through impact testing. Frequency dependence on the hydrothermal conditions was disclosed by testing the sample at different temperatures and with different moisture contents. Based on the frequency measurements, a method was developed to predict the longitudinal Young's modulus and the transverse shear modulus of the sample. The process involves iterative tuning of the moduli of a Timoshenko beam model via a stable characterization scheme. Numerical sensitivity study shows that the moduli thus determined are insensitive to measurement errors rendering the method a possible supplement for conventional static tests. Both frequencies and moduli of the beam sample were found to exhibit an increasing trend with reducing temperature. Besides, freezing of the absorbed moisture enlarged the longitudinal Young's modulus of the material in a significant manner.     

Immunogold FIB‐SEM: Combining Volumetric Ultrastructure Visualization with 3D Biomolecular Analysis to Dissect Cell–Environment Interactions

Volumetric imaging techniques capable of correlating structural and functional information with nanoscale resolution are necessary to broaden the insight into cellular processes within complex biological systems. The recent emergence of focused ion beam scanning electron microscopy (FIB‐SEM) has provided unparalleled insight through the volumetric investigation of ultrastructure; however, it does not provide biomolecular information at equivalent resolution. Here, immunogold FIB‐SEM, which combines antigen labeling with in situ FIB‐SEM imaging, is developed in order to spatially map ultrastructural and biomolecular information simultaneously. This method is applied to investigate two different cell–material systems: the localization of histone epigenetic modifications in neural stem cells cultured on microstructured substrates and the distribution of nuclear pore complexes in myoblasts differentiated on a soft hydrogel surface. Immunogold FIB‐SEM offers the potential for broad applicability to correlate structure and function with nanoscale resolution when addressing questions across cell biology, biomaterials, and regenerative medicine.     

Transverse shear modulus and strength of honeycomb cores

The transverse shear mechanical behavior and failure mechanism of aluminum alloy honeycomb cores are investigated by the single block shear test in this paper. The transverse shear deformation process of honeycomb cores may be approximately categorized into four stages, namely elastic deformation, plastic deformation, fracture of cell walls and debonding of honeycomb cores/facesheets. The elastic deformation of unit cell under transverse shear displacement is also investigated by the finite element method, and the result shows that the bending deformation of the cell walls is similar to that of the cantilever beam. In order to precisely predict the equivalent transverse shear modulus and strength, not only shear deformation but also bending deformation of cell walls should be considered. Therefore, in the present paper, the equivalent transverse shear modulus and strength are predicted by application of the cantilever beam theory and thin plate shear buckling theory in conjunction with simplifying assumption as to the displacement in the cores. It is concluded that the contribution of bending deformation of cell walls to equivalent transverse shear modulus and strength is obvious with the decreasing height of cell walls.     

Characterization of temperature-dependent tensile and flexural rigidities of a cross-ply thermoplastic lamina with implementation into a forming model

This paper discusses the characterization of temperature-dependent tensile and flexural rigidities for Dyneema® HB80, a cross-ply thermoplastic lamina. The low coefficient of friction of this material posed a challenge to securing specimens during tensile testing. Therefore, modification to the standard gripping method was implemented to facilitate the collection of meaningful test data. Furthermore, a long gauge length was selected to moderate the influence of slippage on the measure of the elastic modulus. A new experimental setup is presented to characterize the bending behavior at elevated-temperature conditions based on the vertical cantilever method. The material properties derived from the test data were implemented in a finite element model of the cross-ply lamina. The finite element model is generated using a hybrid discrete mesoscopic approach, and deep-draw forming of the material is simulated to investigate its formability. Simulation results are compared with an experimental forming trial to demonstrate the capabilities of the model to predict the development of out-of-plane waves during preform manufacturing.     

基于声-超声技术的木材弹性模量测定方法研究

提取声信号基频是声-超声方法测定木材弹性模量的关键。由于噪声和传感器谐振频率等因素的影响,直接应用快速傅里叶变换（FFT）方法提取信号基频计算弹性模量通常比标准的力学方法大20%左右。基于此,提出应用最大公约数算法提取信号基频,构建一种测量木材弹性模量的改进方法,并给出此算法的详细步骤。应用该方法和FFT方法分别对杨树木芯样本进行测试,弹性模量Eu和Ef的计算值范围分别为8.23~40.32Gpa和7.94~51.87Gpa,对比标准力学方法（弹性模量Es测量值为6.72~36.35Gpa）,误差下降了约10%。进一步分析Eu-Es和Ef-Es的相关性,相关系数分别为0.94和0.86,都呈显著相关。实测数据表明,应用本文方法计算所得的木材弹性模量与力学方法测试的数值更加吻合,相关性更好。     

First evidence of tyre debris characterization at the nanoscale by focused ion beam

In this paper, we present a novel technique for the nanoscale characterization of the outer and inner structure of tyre debris.

Tyre debris is produced by the normal wear of tyres. In previous studies, the microcharacterization and identification were performed by analytical electron microscopy. This study is a development of the characterization of surface and microstructure of tyre debris. For the first time, tyre debris was analysed by focused ion beam (FIB), a technique with 2- to 5-nm resolution that does not require any sample preparation. We studied tyre debris produced in the laboratory. We made electron and ionic imaging of the surface of the material, and after a ionic cut, we studied the internal microstructure of the same sample. The tyre debris was analysed by FIB without any sample preparations unlike the case of scanning and transmission electron microscopy (SEM and TEM). Useful information was derived to improve detection and monitoring techniques of pollution by tyre degradation processes.     

高频热压杨木单板层积材纵向弹性模量和泊松比的测定与分析

基于四点弯曲法,对一种基于高频热压技术的厚型杨木单板层积材的纵向弹性模量和纵横向泊松比进行了试验测定。其中纵向弹性模量的测定,分别采用了挠度法和应变片法。实验结果表明,2种测量方法所得纵向弹性模量数值比较接近,但又存在一定的差异,并对其差异的影响因素进行了探讨。基于高频热压技术的杨木单板层积材纵向弹性模量的测定结果表明,其纵向弹性模量接近甚至超过杨木单板,为该材料引入重型产品包装箱领域甚至结构用材料,从而替代原木,提供了一定的参考价值。     

Dynamic fracture of a beam or plate under tensile loading

The dynamic fracture response of a long beam of brittle elastic material under tensile loading is studied. If the magnitude of the applied loading is increased to a critical value, a crack is assumed to propagate across the beam cross section. In a parallel analysis to [t] the crack length and applied loading at the fracture face are determined as functions of time measured from fracture initiation. The results of the analysis are shown in graphs of crack length, crack tip speed and fracturing section tensile loading vs time. As found in [1], the crack tip accelerates very quickly to a speed near the characteristic terminal speed for the material, travels at this speed through most of the beam thickness, and then decelerates rapidly in the final stage of the process. Finally, by appropriate change of the elastic modulus, the results may be applied to plane strain fracture of a plate under pure tensile loading.     

A method to quantitatively measure the elastic modulus of materials in nanometer scale using atomic force microscopy

A method is proposed for quantitatively measuring the elastic modulus of materials using atomic force microscopy (AFM) nanoindentation. In this method, the cantilever deformation and the tip-sample interaction during the early loading portion are treated as two springs in series, and based on Sneddon's elastic contact solution, a new cantilever-tip property α is proposed which, together with the cantilever sensitivity A, can be measured from AFM tests on two reference materials with known elastic moduli. The measured α and A values specific to the tip and machine used can then be employed to accurately measure the elastic modulus of a third sample, assuming that the tip does not get significantly plastically deformed during the calibration procedure. AFM nanoindentation tests were performed on polypropylene (PP), fused quartz and acrylic samples to verify the validity of the proposed method. The cantilever-tip property and the cantilever sensitivity measured on PP and fused quartz were 0.514?GPa and 51.99?nm?nA(-1), respectively. Using these measured quantities, the elastic modulus of acrylic was measured to be 3.24?GPa, which agrees well with the value measured using conventional depth-sensing indentation in a commercial nanoindenter.     

Closed-form solutions for axially functionally graded Timoshenko beams having uniform cross-section and fixed–fixed boundary condition

In this paper, we study the free vibration of axially functionally graded (AFG) Timoshenko beams, with uniform cross-section and having fixed–fixed boundary condition. For certain polynomial variations of the material mass density, elastic modulus and shear modulus, along the length of the beam, there exists a fundamental closed form solution to the coupled second order governing differential equations with variable coefficients. It is found that there are an infinite number of non-homogeneous Timoshenko beams, with various material mass density, elastic modulus and shear modulus distributions having simple polynomial variations, which share the same fundamental frequency. The derived results can be used as benchmark solutions for testing approximate or numerical methods used for the vibration analysis of non-homogeneous Timoshenko beams. They can also be useful for designing fixed–fixed non-homogeneous Timoshenko beams which may be required to vibrate with a particular frequency.     

Analysis of creep and modulus loss of the wood cell wall

This paper proposes a nonlinear constitutive model for the wood cell wall based on the nonequilibrium thermodynamics. The wood cell wall is modeled as a long fiber-reinforced composite with cellulose microfibril enclosed by hemicellulose and lignin. An internal variable is introduced into the Helmholtz free energy of the cell wall system, to describe the modulus loss of hemicellulose due to moisture absorption. The viscoelastic behavior of the wood cell wall changes with its moisture content, which leads to different creep evolutions even under the same loading level. To account for this phenomenon, another internal variable is introduced to depict the creep behavior of the wood cell wall, which is correlated with the irreversible energy dissipation processes such as stick–slip mechanism in the wood cell wall. Based on five elastic coefficients of transverse isotropy predicted by the present model, the creep behaviors of the wood cell wall with different microfibril angles are theoretically analyzed and show good agreements with experiment results.     

含裂纹悬臂梁的振动与疲劳耦合分析

基于Paris方程和同步分析方法考虑振动与疲劳裂纹扩展耦合之影响,提出一种含裂纹梁的振动疲劳寿命分析思路.振动分析过程中,利用线性弹簧等效裂纹段,复弹性模量引入阻尼损耗因子,得到考虑裂纹扩展、激励频率和阻尼等因素影响的动应力响应.结果表明:裂纹扩展、激励频率和阻尼等因素对疲劳寿命具有重要的影响.通过振动分析与疲劳裂纹扩展寿命估算同步进行,可进一步提高疲劳寿命估算精度.     

高量程MEMS加速度计灌封后的动态响应

对双悬臂梁高量程MEMS加速度传感器的封装结构进行了1×105g峰值的半正弦加速度冲击载荷下的有限元响应分析。灌封胶弹性模量的变化对加速度计的输出信号(输出电压、悬臂梁的挠度)的影响可以忽略。输出电压曲线的峰值与解析解接近。加速度计的悬臂梁表现为有阻尼下的受迫振动,并表现出悬臂梁的固有频率特性。输出信号的峰值与加速度载荷的峰值均呈很好的线性关系。灌封胶的弹性模量大于4GPa时胶已经足够硬,适宜用于保护芯片。