Mechanical elasticity of vapour-liquid-solid grown GaN nanowires

Mechanical elasticity of hexagonal wurtzite GaN nanowires with hexagonal cross sections grown through a vapour-liquid-solid (VLS) method was investigated using a three-point bending method with a digital-pulsed force mode (DPFM) atomic force microscope (AFM). In a diameter range of 57-135?nm, bending deflection and effective stiffness, or spring constant, profiles were recorded over the entire length of end-supported GaN nanowires and compared to the classic elastic beam models. Profiles reveal that the bending behaviour of the smallest nanowire (57.0?nm in diameter) is as a fixed beam, while larger nanowires (89.3-135.0?nm in diameter) all show simple-beam boundary conditions. Diameter dependence on the stiffness and elastic modulus are observed for these GaN nanowires. The GaN nanowire of 57.0?nm diameter displays the lowest stiffness (0.98?N?m(-1)) and the highest elastic modulus (400 ± 15?GPa). But with increasing diameter, elastic modulus decreases, while stiffness increases. Elastic moduli for most tested nanowires range from 218 to 317?GPa, which approaches or meets the literature values for bulk single crystal and GaN nanowires with triangular cross sections from other investigators. The present results together with further tests on plastic and fracture processes will provide fundamental information for the development of GaN nanowire devices.     

AFM indentation method used for elastic modulus characterization of interfaces and thin layers

Atomic force microscopy (AFM) is increasingly being used as a nanoindentation tool to measure local elastic properties of surfaces. In this article, a method based on AFM in force volume (force curve mapping) mode is employed to measure the elastic modulus distribution at the interface of a glass flake-reinforced polypropylene sample and at a lead-free Cu–solder joint. Indentation arrays are performed using a diamond AFM tip. The processing of experimental AFM indentation data is automated by customized software that can analyse and calibrate multiple force curves. The analysis algorithm corrects the obtained force curves by selecting the contact point, discarding the non-contact region and subtracting the cantilever deflection from the measured force curve in order to obtain true indentation curves. A Hertzian model is then applied to the resulting AFM indentation data. Reference materials are used to estimate the tip radius needed to extract the elastic modulus values. With the proposed AFM measurement method, we are able to obtain high-resolution maps showing elastic modulus variations around a composite interface and a Cu–solder joint. No distinct interphase region is detected in the composite case, whereas a separate intermetallic layer (1–2 μm thick) of much higher Young’s modulus (~131 GPa) than Cu and solder material is identified in the Cu–solder joint. Elastic modulus results obtained for the Cu (~72 GPa), solder (~50 GPa) and glass (~65 GPa) materials are comparable to the results obtained by instrumented indentation [~73, ~46 and ~61 GPa], which accentuates the potential of this method for applications requiring high lateral resolution.     

Mapping the elastic properties of granular Au films by contact resonance atomic force microscopy

Endowed with nanoscale spatial resolution, contact resonance atomic force microscopy (CR-AFM) provides extremely localized elastic property measurements. We advance here the applicability of CR-AFM on surfaces with nanosize features by considering the topography contribution to the CR-AFM signal. On nanosize granular Au films, the elastic modulus at the grain scale has been mapped out by considering a self-consistent deconvolution of the contact geometry effect in the CR-AFM image. Significant variation in the contact area over granular topography arises as the probe is either in single-?or multiple-asperity contact with the surface. Consequently, in extracting the elastic modulus from CR-AFM measurements on granular surfaces we considered both the normal and lateral couplings established through multiple-asperity contacts between the tip and the surface. Thus, by appropriately considering the change in the contact mechanics during CR-AFM imaging, variations in the elastic modulus have been revealed in the intergrain regions as well as across individual grains.     

利用原子力显微镜低频声学模式观察氧化锌压敏电阻

介绍在商用原子力显微镜上建立的低频声学成像模式,并利用其对氧化锌压敏电阻陶瓷晶界处进行了弹性性能成像.声学像中晶界处微晶的衬度反映了添加物的分布.而晶界处的衬度增强现象可能说明样品经热处理后发生富铋相的相变.结果显示低频声成像的分辨率达到了纳米量级,在功能材料的微区力学性能表征方面具有良好的应用前景.     

原子力声显微镜的原理及应用

原子力声显微镜结合了超声检测技术的三维成像能力与原子力显微镜的纳米尺度成像的近场显微技术。它在商用的原子力显微镜设备的基础上加以压电超声传感器产生声激励,并使用锁相放大器对数据进行收集分析,既可得到三维的纳米级的清晰形貌图,又能通过建模分析样品表面的接触刚度及样品的弹性模量。目前,原子力显微镜被广泛应用于材料领域,用于检测样品的机械性能,比如样品的接触刚度、薄膜高分子材料的弹性模量,同时还运用于医学生物领域,用于观察细胞的超微结构及其表面和亚表面的弹性模量等。     

Determining Mechanical Properties of Carbon Microcoils Using Lateral Force Microscopy

Mechanical properties of amorphous carbon microcoil (CMC) synthesized by thermal chemical vapor deposition method were examined in compression and tension tests, using the lateral force mode of atomic force microscope (AFM). The AFM cantilever tip was manipulated by a piezoelectric scanner to contact, pull, and push an individual CMC. The lateral force that was exerted by the CMC deformation causes the twist of the AFM cantilever. It was monitored by the laser and photodetector of the AFM during the experiments. A linear response of the CMC was observed in the range of 25 nm to 5 mum of tension experiments. The results show that the spring constant of the CMC is reasonably proportional to the coil number. The shear modulus of the amorphous CMC is estimated to be 3 plusmn 0.2 GPa. The proposed method is promising to manipulate the compression and tension of the CMC and to measure the lateral force exerted in an ambient environment.     

Vertically aligned nanowires from boron-doped diamond

Vertically aligned diamond nanowires with controlled geometrical properties like length and distance between wires were fabricated by use of nanodiamond particles as a hard mask and by use of reactive ion etching. The surface structure, electronic properties, and electrochemical functionalization of diamond nanowires were characterized by atomic force microscopy (AFM) and scanning tunneling microscopy (STM) as well as electrochemical techniques. AFM and STM experiments show that diamond nanowire etched for 10 s have wire-typed structures with 3-10 nm in length and with typically 11 nm spacing in between. The electrode active area of diamond nanowires is enhanced by a factor of 2. The functionalization of nanowire tips with nitrophenyl molecules is characterized by STM on clean and on nitrophenyl molecule-modified diamond nanowires. Tip-modified diamond nanowires are promising with respect to biosensor applications where controlled biomolecule bonding is required to improve chemical stability and sensing significantly.     

Microstructure-hardened silver nanowires

To exploit the novel size-dependent mechanical properties of nanowires, it is necessary for one to develop strategies to control the strength and toughness of these materials. Here, we report on the mechanical properties of silver nanowires with a unique fivefold twin structure using a lateral force atomic force microscopy (AFM) method in which wires are held in a double-clamped beam configuration. Force-displacement curves exhibit super elastic behavior followed by unexpected brittle failure without significant plastic deformation. Thermal annealing resulted in a gradual transition to weaker, more ductile materials associated with the elimination of the twinned boundary structure. These results point to the critical roles of microstructure and confinement in engineering the mechanical properties of nanoscale materials.     

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.     

The role of substrate surface alteration in the fabrication of vertically aligned CdTe nanowires

Previously we have described the deposition of vertically aligned wurtzite CdTe nanowires derived from an unusual catalytically driven growth mode. This growth mode could only proceed when the surface of the substrate was corrupted with an alcohol layer, although the role of the corruption was not fully understood. Here, we present a study detailing the remarkable role that this substrate surface alteration plays in the development of CdTe nanowires; it dramatically improves the size uniformity and largely eliminates lateral growth. These effects are demonstrated to arise from the altered surface's ability to limit Ostwald ripening of the catalytic seed material and by providing a surface unable to promote the epitaxial relationship needed to sustain a lateral growth mode. The axial growth of the CdTe nanowires is found to be exclusively driven through the direct impingement of adatoms onto the catalytic seeds leading to a self-limiting wire height associated with the sublimation of material from the sidewall facets. The work presented furthers the development of the mechanisms needed to promote high quality substrate-based vertically aligned CdTe nanowires. With our present understanding of the growth mechanism being a combination of selective area epitaxy and a catalytically driven vapour-liquid-solid growth mode, these results also raise the intriguing possibility of employing this growth mode in other material systems in an effort to produce superior nanowires.     

Multiple cracking in aligned polypropylene fibre reinforced cement composites

Multiple cracking has been shown to occur in hardened cement paste reinforced with aligned polypropylene fibres of elastic modulus considerably lower than that of the cement paste. The effect of fibre volume fraction on the distribution of matrix cracks has been studied and good agreement found with existing theory. Factors which enable fibre/matrix contact to be maintained during the multiple cracking process, despite the unfavourable Poisson's ratio contraction of polypropylene have been discussed. These include the lateral displacement of one surface of a crack relative to the other and also the lateral displacement of matrix material next to the crack surface relative to the fibre array. This latter mechanism is shown to apply to other aligned composites and calculations based on a simple theory predict that multiple cracking should occur in all composites provided that a critical size is exceeded.     

Mechanical characterization of nickel nanowires by using a customized atomic force microscope

A new experimental method to characterize the mechanical properties of metallic nanowires is introduced. An accurate and fast mechanical characterization of nanowires requires simultaneous imaging and testing of the nanowires. However, existing mechanical characterization techniques fail to accomplish this goal due either to the lack of imaging capability of the mechanical test setup or the difficulty of individual alignment and manipulation of single nanowires for each test. In this study, nanowire specimens prepared by an electroplating technique are located on a silicon substrate with trenches. A customized atomic force microscope is located inside a scanning electron microscope (SEM) in order to establish the visibility of the nanowires, and the tip of the atomic force microscope cantilever is utilized to bend and break the nanowires. The ability to visualize the nanowires in an SEM improves the speed and accuracy of the tests. Experimentally obtained force versus bending displacement curves are fitted into existing analytical formulations to extract the mechanical properties. Experimental results reveal that nickel nanowires have significantly higher strengths than their bulk counterparts, although their elastic modulus values are comparable to bulk nickel modulus values.     

用于减小控制对测量影响的AFM新工作模式

原子力显微镜（atomic force microscope，AFM）是纳米尺度线宽成像和测量的重要工具．但系统的非线性和控制器参数选择的多样性导致AFM控制的不确定性，影响了AFM测量结果的精确性和重复性．为克服这个缺点，分析了AFM的测量原理和工作模式的特点，在此基础上提出了一种新的工作模式——补偿模式．在这种工作模式中，结合了扫描器和悬臂梁的位置信息而得到被测试样表面的形貌图像．与恒力接触模式相比，在补偿模式下，AFM能够在高速度下以更好的精确性和重复性进行成像和测量．仿真和实验结果证明了这种新工作模式的可行性和适用性．实验结果说明该工作模式可以提高扫描速度16倍或减小均方根误差到约1／5．     

基于AFM纳米硬度测量系统的实验

为了解决用AFM自身压痕软件进行纳米硬度测量时无法直接获得载荷-压深曲线和由于受到扫描陶管扫描范围的限制而进行多点压痕实验范围有限的问题,建立了三维微动工作台和原子力显微镜相结合的纳米压痕硬度测量系统.基于该系统,对单晶薄膜材料进行了单点压痕实验,得出该系统适合进行纳米硬度测量的结论;并对薄膜材料的纳米硬度和弹性模量进行了分析,讨论了尺寸效应对两者的影响.另外,进行了40×40的点阵压痕实验,得到了材料整个压痕面的三维形貌图和三维硬度图.     

In situ observation of size-scale effects on the mechanical properties of ZnO nanowires

In this investigation, the size-scale in mechanical properties of individual [0001] ZnO nanowires and the correlation with atomic-scale arrangements were explored via in situ high-resolution transmission electron microscopy (TEM) equipped with atomic force microscopy (AFM) and nanoindentation (NI) systems. The Young's modulus was determined to be size-scale-dependent for nanowires with diameter, d, in the range of 40 nm ≤ d ≤ 110 nm, and reached the maximum of ～ 249 GPa for d = 40 nm. However, this phenomenon was not observed for nanowires in the range of 200 nm ≤ d ≤ 400 nm, where an average constant Young's modulus of ～ 147.3 GPa was detected, close to the modulus value of bulk ZnO. A size-scale dependence in the failure of nanowires was also observed. The thick ZnO nanowires (d ≥ 200 nm) were brittle, while the thin nanowires (d ≤ 110 nm) were highly flexible. The diameter effect and enhanced Young's modulus observed in thin ZnO nanowires are due to the combined effects of surface relaxation and long-range interactions present in ionic crystals, which leads to much stiffer surfaces than bulk wires. The brittle failure in thicker ZnO wires was initiated from the outermost layer, where the maximum tensile stress operates and propagates along the (0001) planes. After a number of loading and unloading cycles, the highly compressed region of the thinner nanowires was transformed from a crystalline to an amorphous phase, and the region near the neutral zone was converted into a mixture of disordered atomic planes and bent lattice fringes as revealed by high-resolution images.     

Structural,mechanical, and electrical properties of carbon nanoparticles synthesized from diesel

We studied the elemental analysis, structural morphology, mechanical, and electrical properties of carbon nanoparticles synthesized from diesel. The spherical carbon particle size in the range of about 10 to 80 nm in diameter was observed in scanning electron microscope (SEM) studies that were identified by Atomic force microscopy (AFM) study as an aggregation of carbon particles of average size 2.5 nm. The surface rms of carbon nanoparticle thin film (CNTF) was measured directly by AFM and found 0.22 nm. The Derjaguin–Muller–Toporov (DMT) elastic modulus of carbon nanoparticles (CNPs) was measured by PeakForce QNM mode of AFM. The minimum and maximum elastic modulus was measured of 0.40 GPa and 43.89 GPa, respectively. The resistivity, conductivity, magneto resistance, mobility, and average Hall co-efficient were measured by “Ecopia Hall-effect measurement system” by four-point Van der Pauw approach at ambient condition. We demonstrated I–V characteristic at the Indium/CNTF thin film interface, which is accompanied by rectifying behavior.     

原子力声显微镜成像及分析

超声检测技术与原子力显微技术相结合,构成原子力声显微镜(AFAM),能够实现样品内部纳米结构的测量,并分析如局域弹性模量、刚度等力学性能.本文在传统的原子力显微镜(AFM)的基础上初步构建了AFAM,利用AFM轻敲模式下的微悬臂梁振动激励信号来驱动样品背面的压电超声换能器,并利用轻敲模式控制系统中的锁相环检测经过样品后由探针收集的振动信号,形成振幅及相位图像.这种AFAM方法不需外接信号发生器、锁相放大器及相关控制电路,从而避免AFM内、外部的仪器及控制电路的不同步而引起的AFAM振幅/相位与形貌图像间的偏移.此外,还分析了形貌结构对AFAM振幅图像的影响,为进一步研究AFAM亚表面成像奠定了基础.     

Catalyst-free synthesis, structural, and mechanical characterization of twinned Mg2B2O5 nanowires

Mg2B2O5 nanowires with (010) twins were synthesized for the first time using a catalyst-free method. The microstructure of the Mg2B2O5 nanowires has been extensively studied by cross-sectional high-resolution transmission electron microscopy. Nanoindentation tests were performed directly on individual nanowires to probe their mechanical properties. It was found that the twinned Mg2B2O5 nanowires achieve comparable hardness but 19% decrease in elastic modulus compared to their bulk counterpart. The elastic softening mechanisms of the Mg2B2O5 nanowires are discussed with reference to their twin defects, size, and surface effects.     

Measurement of elastic properties of calcium silicate hydrate with atomic force microscopy

Atomic force microscopy (AFM) based indentation is compared to conventional nanoindentation for measuring mechanical properties of cement pastes. In evaluating AFM as a mechanical characterization tool, various analytical and numerical modeling approaches are compared. The disparities between the numerical self-consistent approach and analytical solutions are determined and reported. The measured elastic Young’s modulus determined from AFM indentation tests are compared to elastic Young’s modulus determined from nanoindentation tests of cement paste. These results indicate that the calcium silicate hydrate (C-S-H) phase of hydrated Portland cement has different properties on the different length scales probed by AFM versus nanoindenters. Packing density of C-S-H particles is proposed as an explanation for the disparity in the measured results.     

Deep-learning-based nanowire detection in AFM images for automated nanomanipulation

Atomic force microscope(AFM)-based nanomanipulation has been proved to be a possible method for assembling various nanoparticles into complex patterns and devices.To achieve efficient and fully automated nanomanipulation,nanoparticles on the substrate must be identified precisely and automatically.This work focuses on an autodetection method for flexible nanowires using a deep learning technique.An instance segmentation network based on You Only Look Once version 3(YOLOv3)and a fully convolutional network(FCN)is applied to segment all movable nanowires in AFM images.Combined with follow-up image morphology and fitting algorithms,this enables detection of postures and positions of nanowires at a high abstraction level.Benefitting from these algorithms,our program is able to automatically detect nanowires of different morphologies with nanometer resolution and has over 90%reliability in the testing dataset.The detection results are less affected by image complexity than the results of existing methods and demonstrate the good robustness of this algorithm.