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．     

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.     

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.     

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。     

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、     

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。     

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.     

原子力显微镜下蚕丝及蜘蛛丝的微观结构

利用原子力显微镜研究了蚕丝丝素、蜘蛛牵引丝及其内外层包卵丝的微观结构.研究表明,丝素和包卵丝纤维的纵向表面都有成丝过程中液态丝蛋白流动而形成的清晰的构槽和条纹,在低速下自然分泌的牵引丝的表面皮层相对比较细腻,而垂直下落蜘蛛在高速下分泌的牵引丝具有和丝素纤维比较相似的微观结构特征.这些丝纤维的断面内都分布有大量微细的原纤,形状基本为圆形,其中三种蜘蛛丝的微纤维直径相似,而丝素纤维内的微纤维要粗得多.     

X-Ray Microanalysis in the Variable Pressure (Environmental) Scanning Electron Microscope

Electron-excited x-ray microanalysis performed in the variable pressure and environmental scanning electron microscopes is subject to additional artifacts beyond those encountered in the conventional scanning electron microscope. Gas scattering leads to direct contributions to the spectrum from the environmental gas, as well as remote generation of x rays by electrons scattered out of the focussed beam. The analyst can exert some degree of control over these artifacts, but depending on the exact situation, spurious elements can appear at the trace (< 0.01 mass fraction), minor (0.01 mass fraction to 0.1 mass fraction), or even major (> 0.1 mass fraction) levels. Dispersed particle samples give the least compromised results, while fine scale microstructures are the most severely compromised. Procedures to optimize the situation based upon specimen preparation as well as spectral processing are described.     

Characterization of Probe Dynamic Behaviors in Critical Dimension Atomic Force Microscopy

This paper describes a detailed computational model of the interaction between an atomic force microscope probe tip and a sample surface. The model provides analyses of dynamic behaviors of the tip to estimate the probe deflections due to surface intermittent contact and the resulting dimensional biases and uncertainties. Probe tip and cantilever beam responses to intermittent contact between the probe tip and sample surface are computed using the finite element method. Intermittent contacts with a wall and a horizontal surface are computed and modeled, respectively. Using a 75 nm Critical Dimension (CD) tip as an example, the responses of the probe to interaction forces between the sample surface and the probe tip are shown in both time and frequency domains. In particular, interaction forces between the tip and both a vertical wall and a horizontal surface of a silicon sample are modeled using Lennard-Jones theory. The Snap-in and Snap-out of the probe tip in surface scanning are calculated and shown in the time domain. Based on the given tip-sample interaction force model, the calculation includes the compliance of the probe and dynamic forces generated by an excitation. Cantilever and probe tip deflections versus interaction forces in the time domain can be derived for both vertical contact with a plateau and horizontal contact with a side wall. Dynamic analysis using the finite element method and Lennard-Jones model provide a unique means to analyze the interaction of the probe and sample, including calculation of the deflection and the gap between the probe tip and the measured sample surface.     

原子力显微镜在材料研究中的应用

简述原子力显微镜的工作原理及特点,以实例介绍其在材料研究中的应用,指出原子力显微镜在材料的研究过程中有广阔的应用前景。     

The Analysis of Particles at Low Accelerating Voltages (≤ 10 kV) With Energy Dispersive X-Ray Spectroscopy (EDS)

In recent years, there have been a series of advancements in electron beam instruments and x-ray detectors which may make it possible to improve significantly the quality of results from the quantitative electron-probe analysis of individual particles. These advances include: (1) field-emission gun electron beam instruments such as scanning electron microscopes (FEG-SEMs) that have high brightness electron guns with excellent performance at low beam energies, E₀ ≤ 10 keV and (2) high-resolution energy-dispersive x-ray spectrometers, like the microcalorimeter detector, that provide high-resolution (< 10 eV) parallel x-ray collection. These devices make it possible to separate low energy (< 4 keV) x-ray lines including the K lines of carbon, nitrogen and oxygen and the L and M lines for elements with atomic numbers in the range of 25 to 83. In light of these advances, this paper investigates the possibility of using accelerating voltages ≤ 10 kV, as a method to improve the accuracy of elemental analysis for micrometer-sized particles.     

Voltage contrast studies on 0·5 μm integrated circuits by scanning force microscopy

A scanning force microscope (SFM) test system is used for voltage contrast studies on 0·5 μm integrated circuits. Waveform measurements are performed on passivated 0·5 μm conducting lines up to 4 GHz. Additionally two-dimensional measurements at 10 MHz demonstrate the potential for device internal function and failure analysis in the sub-μm regime by direct correlation between voltage contrast and quantitative topography images.     

Electron and Atomic Force Microscopy studies of photocatalytic titanium dioxide thin films deposited by DC magnetron sputtering

Titanium dioxide thin films were deposited on glass substrates and on fluorine doped tin oxides at room temperature by DC magnetron sputtering at different working gas pressures and were evaluated using photocatalytic degradation of an organic compound. The structural properties of the films were studied by electron microscopy techniques and Atomic Force Microscopy. Numerous structural defects were detected for samples deposited at 16 mTorr and it was associated with the highest photo-degradation rate. Also small band gap shift in titanium dioxide films was detected for different gas pressures. These behaviors are related with structural details derived from the synthesis conditions and the influence of structural defects on the photocatalytic activity is discussed.     

半金属铋薄膜导电特性和粗糙度的研究

本论文利用真空镀膜方法在云母片上生长半金属Bi薄膜,测量了薄膜生长厚度与电阻之间的关系,并用原子力显微镜(AFM)研究了云母表面半金属薄膜电阻变化与薄膜粗糙度间的关系.生长初始阶段,薄膜先形成孤立的三维小岛(典型高度1 nm,直径10 nm,间距10 nm),随后互相聚结形成网状结构,薄膜不导通(R≥20 MΩ),粗糙度随膜厚增加而减小.当等效厚度d=1.74 nm时,薄膜导通(R≤13 MΩ),薄膜的形貌变为有小孔洞的连续状结构,粗糙度在此厚度附近达到最小值然后又增大.随着薄膜继续生长,连续状结构的厚度增加,薄膜电阻随之迅速减小,当d≥2.4 nm时薄膜电阻趋近于稳定值2kΩ.     

利用计量型原子力显微镜进行纳米台阶高度测量

计量型原子力显微镜纳米测量系统主要由扫描器、测针位置传感器和一体化微型激光干涉三维测量系统等部分构成．针对计量型原子力显微测量系统,采用三维激光干涉测量系统作为测量基准,以实现原子力测量系统的纳米尺度量值溯源和校准工作．建立了校准模型,分析了扫描器9项主要误差项,并将该模型应用到原子力显微镜扫描器的校准中．校准后的结果表明,除z轴位置误差不超过±2nm外,其他8项的残余误差均不超过±1nm．通过台阶高度国际比对,建立了台阶高度标准计算方法及不确定度分析模型．台阶高度国际比对的测量结果表明,计量型原子力显微镜的测量值与参考值相差均小于1．5nm．     

Optical Calibration of a Submicrometer Magnification Standard

The calibration of a new submicrometer magnification standard for electron microscopes is described. The new standard is based on the width of a thin thermal-oxide film sandwiched between a silicon single-crystal substrate and a polysilicon capping layer. The calibration is based on an ellipsometric measurement of the oxide thickness before the polysilicon layer is deposited on the oxide. The uncertainty in the derivation of a thickness for the layer from the ellipsometric parameters is also derived.