基于AFM的纳米级表面加工中切屑形成的影响因素

以原子力显微镜（AFM）为加工工具进行了纳米级加工实验,对不同加工条件下的材料去除过程和切屑形态进行了研究．切屑形态通过扫描电子显微镜（SEM）进行观察,分析了不同垂直载荷、循环次数和针尖加工方向下铝铜被加工表面的切屑形成过程．实验结果表明：低栽下切屑呈细小断屑,散布在加工区域周围;随着垂直载荷的增加,切屑逐渐变成连续的带状切屑．不同循环次数、针尖加工面时切屑形成都有很大影响．在此基础上,对比分析了相同实验条件下,不同力学性能材料的切屑形成过程．最后,通过检测被加工表面得出被加工表面质量与切屑的数量和形态之间的关系,提出了改善被加工表面质量的方法,以帮助人们更好地理解基于AFM的纳米级加工技术．     

Opportunities in High‐Speed Atomic Force Microscopy

The atomic force microscope (AFM) has become integrated into standard characterisation procedures in many different areas of research. Nonetheless, typical imaging rates of commercial microscopes are still very slow, much to the frustration of the user. Developments in instrumentation for “high‐speed AFM” (HSAFM) have been ongoing since the 1990s, and now nanometer resolution imaging at video rate is readily achievable. Despite thorough investigation of samples of a biological nature, use of HSAFM instruments to image samples of interest to materials scientists, or to carry out AFM lithography, has been minimal. This review gives a summary of different approaches to and advances in the development of high‐speed AFMs, highlights important discoveries made with new instruments, and briefly discusses new possibilities for HSAFM in materials science.     

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.     

Quantification of Lubricant Activity of Magnesium Stearate by Atomic Force Microscopy

Magnesium stearate (MgSt) is commonly used in pharmaceutical formulations as a lubricant to facilitate tablet release from the die after compression. In this study, we quantify the effect of MgSt on the interaction forces between microcrystalline cellulose (MCC) and steel surfaces. A quantitative approach to better understand the mechanism by which MgSt affects powder performance will assist in improved control and formulation design. We find that the forces between MgSt and steel surface are stronger than the interactions between MgSt itself, between MgSt and an MCC particle, and an MCC particle and a steel surface. These quantitative findings offer an explanation how MgSt facilitates lubrication during tablet ejection.     

Long Jumps of an Organic Molecule Induced by Atomic Force Microscopy Manipulation

Non‐contact atomic force microscopy at cryogenic temperatures is used for the controlled lateral manipulation of individual 3,4,9,10‐perylene‐tetracarboxylicacid‐dianhydride (PTCDA) molecules on the Ag(111) surface. The molecules are moved along the [‐110] direction of the Ag lattice in the regime of repulsive tip‐molecule forces performing discrete jumps that span distances from single to multiple lattice spacings. The analysis of the two‐dimensional force field measured before and during the manipulation reveals that the displacement beyond nearest neighbor sites cannot be explained by long range tip‐molecule forces but instead has to involve an energy transfer to translational modes of the molecule. Combined with the results of the simultaneous measurement of the energy dissipation, these findings allow to identify a likely manipulation mechanism and provide insight into the process of energy transfer between excited large molecules and metal surfaces. Furthermore, implications for the theoretical treatment of NC‐AFM based molecule manipulation are discussed.     

Nanomanipulation by Atomic Force Microscopy

The linking of our macroscopic world to the nanoscopic world of single molecules, nanoparticles and functional nanostructures is a technological challenge. Researchers in nanobiotechnology face the questions “How extract and analyze a single nano‐object?”, “How to pick and place nano‐objects?” and “How to prototype a functional nanostructure?”. Here, nanomanipulation by an atomic force microscope (AFM) in combination with optical manipulation by a microbeam laser offers a practicable solution. In such a system, the AFM can be operated as a nanorobot for manipulation purposes allowing for nanometer precision. A contact free manipulation is achieved by the laser microbeam.     

Barriers to Quantitative Electron Probe X-Ray Microanalysis for Low Voltage Scanning Electron Microscopy

Low voltage x-ray microanalysis, defined as being performed with an incident beam energy ≤5 keV, can achieve spatial resolution, laterally and in depth, of 100 nm or less, depending on the exact selection of beam energy and the composition of the target. The shallow depth of beam penetration, with the consequent short path length for x-ray absorption, and the low overvoltage, the ratio of beam energy to the critical ionization energy, both contribute to minimizing the matrix effects in quantitative x-ray microanalysis when the unknown is compared to pure element standards. The low beam energy restricts the energy of the atomic shells that can be excited, forcing the analyst to choose unfamiliar shells/characteristic peaks. The low photon energy shells are subject to low fluorescence yield, so that the peak-to-continuum background is reduced, severely limiting detectability. The limited resolution of semiconductor energy dispersive spectrometry results in frequent peak interference situations and further exacerbates detection limits. Future improvements to the x-ray spectrometry limitations are possible with x-ray optics-augmented wavelength dispersive spectrometry and microcalorimeter energy dispersive spectrometry.     

具有溯源性的原子力显微镜探针法向弹性常数标定系统

原子力显微镜(AFM)悬臂梁探针的弹性常数在微纳米尺度力学测试中十分重要,其准确程度直接影响力学测量结果的可靠性,故需对其进行精确标定.因天平法的测量结果可溯源,本文在已有天平法的基础上,研制了一套新型标定系统.该系统将AFM测头与超精密电磁天平相结合.微悬臂梁在精密位移台的带动下接触天平并产生弯曲,接触力由天平测得,微悬臂梁的弯曲量由光杠杆检测,并通过反馈系统进行精确控制,最后根据胡克定律计算出弹性常数.利用本系统对4种不同型号商用微悬臂梁探针的法向弹性常数进行了标定,标定结果表明本系统具有良好的测量重复性.通过进行不确定度分析,得到测量结果的相对标准不确定度优于2%.     

Detection of Single DNA Molecule Hybridization on a Surface by Atomic Force Microscopy

Improving the detection of DNA hybridization is a critical issue for several challenging applications encountered in microarray and biosensor domains. Herein, it is demonstrated that hybridization between complementary single‐stranded DNA (ssDNA) molecules loosely adsorbed on a mica surface can be achieved thanks to fine‐tuning of the composition of the hybridization buffer. Single‐molecule DNA hybridization occurs in only a few minutes upon encounters of freely diffusing complementary strands on the mica surface. Interestingly, the specific hybridization between complementary ssDNA is not altered in the presence of large amounts of nonrelated DNA. The detection of single‐molecule DNA hybridization events is performed by measuring the contour length of DNA in atomic force microscopy images. Besides the advantage provided by facilitated diffusion, which promotes hybridization between probes and targets on mica, the present approach also allows the detection of single isolated DNA duplexes and thus requires a very low amount of both probe and target molecules.     

Fluidic Force Microscopy and Atomic Force Microscopy Unveil New Insights into the Interactions of Preosteoblasts with 3D-Printed Submicron Patterns

Physical patterns represent potential surface cues for promoting osteogenic differentiation of stem cells and improving osseointegration of orthopedic implants. Understanding the early cell–surface interactions and their effects on late cellular functions is essential for a rational design of such topographies, yet still elusive. In this work, fluidic force microscopy (FluidFM) and atomic force microscopy (AFM) combined with optical and electron microscopy are used to quantitatively investigate the interaction of preosteoblasts with 3D-printed patterns after 4 and 24 h of culture. The patterns consist of pillars with the same diameter (200 nm) and interspace (700 nm) but distinct heights (500 and 1000 nm) and osteogenic properties. FluidFM reveals a higher cell adhesion strength after 24 h of culture on the taller pillars (32 ± 7 kPa versus 21.5 ± 12.5 kPa). This is associated with attachment of cells partly on the sidewalls of these pillars, thus requiring larger normal forces for detachment. Furthermore, the higher resistance to shear forces observed for these cells indicates an enhanced anchorage and can be related to the persistence and stability of lamellipodia. The study explains the differential cell adhesion behavior induced by different pillar heights, enabling advancements in the rational design of osteogenic patterns.     

用原子力显微镜研究葡聚糖包覆纳米氧化铁微粒的形貌特征

采用化学共沉淀法合成了葡聚糖包覆的超顺磁纳米氧化铁微粒,用原子力显微镜对其分布状态、微粒形貌和尺度等进行了表征,并与透射电镜观察结果进行了比较。结果表明：葡聚糖包覆的超顺磁纳米氧化铁微粒大小均匀且有规律的定向分布,无团聚现象;透射电镜显示其核心氧化铁纳米粒子的外形主要为不规则的球形,粒径5～20nm被葡聚糖包覆后的纳米氧化铁微粒呈长方体,尺寸为（200-300）nm×（400-600）nm×（50-70）nm。     

用于双探针原子力显微镜的定位平台的设计及实验验证

针对双探针原子力显微镜的需求,设计了一种提供精确位移的大行程定位平台。采用柔性铰链和压电陶瓷致动器分别作为定位平台的导向机构和驱动机构。在 X、Y和Z轴运动方向通过并联机构实现独立位移。对定位平台进行数学建模,分析和计算定位平台的工作刚度和固有频率,并进行了有限元仿真分析。以电容传感器作为位移测量单元构建了定位平台实验装置,并进行了实验验证。实验结果表明:定位平台在X与Y轴方向上拥有 110μm 的行程,分辨率为5nm,在Z轴方向上拥有45μm的行程,分辨率为5nm。     

采用原子力显微镜表征羟基磷灰石的形貌

为研究人工合成羟基磷灰石粉体在烧结过程中的表面形貌和粒度的演变,采用X射线衍射和原子力显微镜等手段,研究羟基磷灰石粉末的压制样品在高温炉中经不同温度下烧结后的颗粒形貌和粒度的变化。结果表明,烧结温度和烧结时间对表面形貌和晶粒粒径演变都有影响,而且晶粒粒径符合粒径长大的物理机制。     

原子力显微镜中微悬臂梁/探针横向力的标定

利用微加工制造的微悬臂梁／探针尖已经广泛应用在微观表面性质测试和微纳米尺度加工等领域，成为微纳米研究领域中不可缺少的重要工具．为了能够定量研究原子力显微镜中探针与表面的相互作用力，需要对微悬臂梁／探针的力学性能进行表征．本文简要地论述了原子力显微镜中微悬臂梁的形变光反射原理和探针与表面的接触刚度理论．阐明了微悬臂梁横向力标定的重要性．综述了目前几种微悬臂梁／探针横向力的标定方法、简单的推倒过程和特点、     

Variable Magnification With Kirkpatrick-Baez Optics for Synchrotron X-Ray Microscopy

We describe the distinction between the operation of a short focal length x-ray microscope forming a real image with a laboratory source (convergent illumination) and with a highly collimated intense beam from a synchrotron light source (Köhler illumination). We demonstrate the distinction with a Kirkpatrick-Baez microscope consisting of short focal length multilayer mirrors operating at an energy of 8 keV. In addition to realizing improvements in the resolution of the optics, the synchrotron radiation microscope is not limited to the usual single magnification at a fixed image plane. Higher magnification images are produced by projection in the limit of geometrical optics with a collimated beam. However, in distinction to the common method of placing the sample behind the optical source of a diverging beam, we describe the situation in which the sample is located in the collimated beam before the optical element. The ultimate limits of this magnification result from diffraction by the specimen and are determined by the sample position relative to the focal point of the optic. We present criteria by which the diffraction is minimized.     

扫描Kelvin探针力显微镜:工作原理及在材料腐蚀研究中的应用

扫描Kelvin探针力显微镜(SKPFM)是在原子力显微镜(AFM)的基础上应用扫描Kelvin探针(SKP)技术开发的检测表征手段,它能够在获取材料表面纳米级分辨率形貌的同时,原位得到样品表面高分辨率的接触电势差分布图,为揭示腐蚀反应机理提供了崭新的思路,近年来发展迅速。本文介绍了SKPFM两种工作模式的基本原理,总结了SKPFM在应用中的问题,并讨论了SKPFM和传统扫描Kelvin探针技术(SKP)的优缺点,重点综述了SKPFM在腐蚀科学研究中的应用,最后展望了SKPFM的发展方向与应用前景。