Magnetic refinement of tips for magnetic force microscopy

Silicon cantilever probes with monolithically integrated tips are commercially available and are routinely used for atomic force microscopy (AFM). For such probes, amagnetic refinement of the silicon tip has been developed and results in a deposition of ferromagnetic material such as nickel or CrCoTa in the top area of the tip. The method consists of essentially three steps: (1) A broad-area sputter deposition of a ferromagnetic material; (2) a selective electron beam-induced carbon deposition at the top of the tip; (3) a broad-area ion-beam sputter etching, which removes the magnetic layer everywhere except underneath the carbon cap. The method allows to control the total amount and extension of the magnetic material left at the tip. It is applicable to all kinds of ferromagnetic materials which can be deposited as a thin layer by sputter deposition or evaporation. Experiments indicate that the method is reliable and improves the resolution of magnetic force microscopy (MFM). With such magnetically refined tips on silicon cantilevers, MFM measurements have been performed in contact mode as well as in dynamic and static noncontact modes. In this paper, the method for magnetic tip refinement is described and MFM measurements with these tips are presented.     

Advanced cantilevers for magnetic force microscopy and high frequency magnetic force microscopy

In order to improve the spatial resolution achieved by magnetic force microscopy (MFM) technique and its derivatives, we employ here advanced MFM tips fabricated by means of focused ion beam (FIB) milling. The magnetic coating applied on these tips is a CoCr film of 10 nm thickness. The MFM measurements on hard disk test samples reveal the achieved high resolution, and the measurement on a garnet film demonstrates the low invasiveness. High-frequency MFM (HF-MFM) is a development of the MFM technique to observe the HF stray fields emerging from magnetic recording writer poles at their operating conditions. By means of HF-MFM, magnetic recording writer poles are characterized in the frequency range 100-1,000 MHz. Up to now, all HF-MFM experiments conducted were using standard MFM cantilevers. From the HF-MFM images obtained using the advanced MFM cantilevers, it is clearly seen that the spatial resolution is considerably improved over the images obtained using standard MFM tips. However, the 10 nm thick magnetic coating of the cantilevers is found to work properly only at frequencies of up to about 500 MHz.     

Investigation of Bloch wall fine structures by magnetic force microscopy

Using a magnetic force microscope (MFM), measurements have been performed on single crystal iron whiskers. These samples exhibit a comparatively simple magnetic domain structure and a high degree of crystallographic perfection. STM measurements yield an average surface corrugation of about 3 nm. These nearly ideal boundary conditions permit an investigation of the undistorted surface configuration of Bloch walls in a cubic bulk crystal. Interactions between the stray field configuration of the sample and a ferromagnetic microscope tip have been measured with a new MFM device which is based on direct compliance detection. Measurements have been performed in the constant-current mode, as well as in the constant-compliance, mode. Control observation by means of the Kerr magneto-optic effect permit an interpretation of the obtained MFM data in terms of isolated 180° Bloch walls. The fine structure of these walls has been analysed and compared with results obtained from model calculations.     

In situ study of electric field‐induced magnetization in multiferroic BiFeO3 nanowires

In this work, we have studied electric field‐induced magnetization effect of multiferroic BiFeO₃ (BFO) nanowires in situ using magnetic force microscopy (MFM). Changes in magnetic domain contrast have been observed in the MFM phase images under applied electric potential, which indicate local magnetoelectric (ME) coupling in the nanowires. The values of saturation and magnetization at different applied electric fields were evaluated. These results suggest that one‐dimensional multiferroic BFO nanowires are potential candidates for realizing multiferroic devices at nanoscale with unique functionalities. SCANNING 36:224–230, 2014. © 2013 Wiley Periodicals, Inc.     

Recent advances in magnetic force microscopy

During the past ten years magnetic force microscopy (MFM) has become probably the most powerful general-purpose method for magnetic imaging. MFM can be applied under various environmental conditions and requires only little sample preparation. Basic research on magnetic materials as well as the mentioned industrial applications create an increasing demand for high-resolution magnetic imaging methods. This contribution will review some new concepts which have been realized in the field of advanced probe preparation, based on electron beam methods in order to improve the spatial resolution beyond 100nm. It is shown that the advanced probes allow high-resolution imaging of magnetic fine structures within thin film permalloy elements exhibiting a complicated cooperative magnetization reversal process. These investigations are of importance for various concepts underlying modern magnetic data storage developments. Furthermore, we present some developments of MFM to suit the needs of the magnetic recording industry.     

Atomic force microscopy of a hydrated bacterial surface protein

The protein surface layer of the bacterium Deinococcus radiodurans (HPI layer) was examined with an atomic force microscope (AFM). The measurements on the air-dried, but still hydrated layer were performed in the attractive imaging mode in which the forces between tip and sample are much smaller than in AFM in the repulsive mode or in scanning tunnelling microscopy (STM). The results are compared with STM and transmission electron microscopy (TEM) data.     

Calculation of the Bloch wall contrast in magnetic force microscopy

The magnetic force microscope (MFM) is a promising analytical tool for the mapping of magnetic microfield distributions on a nanometre scale. The detailed interpretation of experimentally obtained data requires a rigorous micromagnetic analysis of the underlying magnetostatic tip-sample interactions. We have performed model calculations yielding the MFM image contrast obtained for 180° Bloch walls using ferromagnetic microscope tips. The actually observed wall image is shown to depend critically upon the mesoscopic tip design. The spatial resolution and also values for the resulting interaction forces and tip-sample compliances are derived.     

Magnetic domain imaging of nano‐magnetic films using magnetic force microscopy with polar and longitudinally magnetized tips

Perpendicular or parallel magnetic fields are used to magnetize the tips used in magnetic force microscopy (MFM). In this process, perpendicular or parallel magnetic dipole moments are produced on the tip plane, thus leading to the formation of polar magnetized tips (PM‐tips) or longitudinally magnetized tips (LM‐tips), respectively. The resolution of an MFM image of a magneto‐optic disk is used for calibration of these tips, and the saturated magnetic fields of the PM‐ and LM‐tips are found to be 2720 Oe and 680 Oe, respectively. Because both tips can simultaneously magnetize the sample during the scanning process when measuring a Co thin film, clear MFM images are captured, which enable the identification of magnetizable regions and the distribution of the magnetic domains on the sample surface. These results will be useful for improving the manufacturing processes required for soft nano‐magnetic film production.     

Calibration of the scanning (atomic) force microscope with gold particles

Scanning force microscopy (SFM) holds great promise for biological research. Two major problems that have confronted imaging with the scanning force microscope have been the distortion of the image and overestimation in measurements of lateral size due to the varying geometry and characteristics of the scanning tip. In this study, spherical colloidal gold particles (10, 20 and 40 nm in diameter) were used to determine (1) tip parameters (size, shape and semivertical angle); (2) the distortion of the image caused by the tip; and (3) the overestimation or broadening of lateral dimensions. These gold particles deviate little in size, are rigid and have a size similar to biological macromolecules. Images of the colloidal gold particles by SFM were compared with those obtained by electron microscopy (EM). The height of the gold particles as measured by SFM and EM was comparable and was little affected by the tip geometry. The measurements of the lateral dimensions of colloidal gold, however, showed substantial differences between SFM and EM in that SFM resulted in an overestimate of the lateral dimensions. Moreover, the distortion of images and broadening of lateral dimensions were specific to the SFM tip used. The calibration of the SFM tip with mica provided little clue as to the type of distortion and the amount of lateral broadening observed when the larger gold particles were scanned. The SFM image also depended on the orientation of the tip with respect to the specimen. Our results suggest that quantitative SFM imaging requires calibration to identify and account for both the distortions and the magnitude of lateral broadening caused by the cantilever tip. Calibration with gold particles is fast and nondestructive to the tip. The raw imaging data of the specimen can be corrected for the tip effect and true structural information can be derived. In summary, we present a simple and practical method for the calibration of the SFM tip using gold particles with a size in the range of biomacromolecules that allows: (1) selection of a cantilever tip that produces an image with minimal distortion; (2) quantitative determination of tip parameters; (3) reconstruction of the shape of the tip at different heights from the tip apex; (4) appreciation of the type of distortion that may be introduced by a specific tip and quantification of the overestimation of the lateral dimensions; and (5) calculation of the true structure of the specimen from the image data. The significance is that such calibration will permit quantitative and accurate imaging with SFM.     

Self-sensing piezoresistive cantilever and its magnetic force microscopy applications

A newly developed Si self-sensing piezoresistive cantilever is presented. Si piezoresistive cantilevers for scanning microscopy are fabricated by Si micro-machining technique. The sensitivity of the piezoresistive cantilever is comparable to the current laser detecting system. Topographic images are successfully obtained with the piezoresistive cantilever and some comparisons are made with the laser detecting system. Furthermore, the magnetic film (Co-Cr-Pt) is coated on the tip of the piezoresistive cantilever for magnetic force microscopy (MFM) application. The magnetic images are successfully obtained with the self-sensing MFM piezoresistive cantilever. The self-sensing piezoresistive cantilevers have been successfully applied in scanning probe microscopy and MFM.     

光学原子力显微镜中的蒙特卡罗方法

扫描探针显微镜(Scanning probe microscopy,SPM)是显微镜的一个分支,它利用物理探针扫描标本形成样本表面图像.而原子力显微镜(Atomic force microscopy,AFM)是SPM中一种多功能的表面成像和测量工具,对导电、不导电、真空中、空气中或流体中的各种样本均可测量.原子力显微镜最面临的最大挑战之一是评估其在表面测量过程中所伴随的不确定度.本研究通过XYZ Phase的标定,对一台光学原子力显微镜进行了校准.该方法旨在克服在评估一些无法实验确定的不确定部件时遇到的困难,如尖端表面相互作用力和尖端几何.运用蒙特卡罗方法来确定根据相关容差和概率密度函数(PDFs)随机绘制参数而引起的相关不确定度.整个过程遵循《测量不确定度表示指南》(GUM)补编2.经本方法验证,原子力显微镜的评估不确定度为10nm左右.     

The tetrahedral tip as a probe for scanning near-field optical microscopy at 30 nm resolution

The tetrahedral tip is introduced as a new type of a probe for scanning near-field optical microscopy (SNOM). Probe fabrication, its integration into a scheme of an inverted photon scanning tunnelling microscope and imaging at 30 nm resolution are shown. A purely optical signal is used for feedback control of the distance of the scanning tip to the sample, thus avoiding a convolution of the SNOM image with other simultaneous imaging modes such as force microscopy. The advantages of this probe seem to be a very high efficiency and its potential for SNOM at high lateral resolution below 30 nm.     

Magnetic field detection for current evaluation by magnetic force microscopy

A current measurement method through magnetic field detection by magnetic force microscopy was proposed and demonstrated. We observed the magnetic field induced by an AC below 2.2 μA around a GaAs/AlGaAs mesa stripe. To achieve high sensitivity in magnetic field detection, we tuned the AC bias frequency to the torsional resonant frequency of the cantilever. As a result, the sensitivity of the magnetic field detection was much improved and specific features of the magnetic field around the mesa stripe were clearly observed at a current in sub-μA range.     

Velocity dependent friction laws in contact mode atomic force microscopy

Friction forces in the tip–sample contact govern the dynamics of contact mode atomic force microscopy. In ambient conditions typical contact radii between tip and sample are in the order of a few nanometers. In order to account for the large interaction area the dynamics of contact mode atomic force microscope (AFM) is investigated under the assumption of a multi-asperity contact interface between tip and sample. Thus, the kinetic friction force between tip and sample is the product of the real contact area between both solids and the interfacial shear strength. The velocity strengthening of the lateral force is modeled assuming a logarithmic relationship between shear-strength and velocity. Numerical simulations of the system dynamics with this empirical model show the existence of two different regimes in contact mode AFM: steady sliding and stick–slip where the tip undergoes periodically stiction and kinetic friction. The state of the system depends on the scan velocity as well as on the velocity dependence of the interfacial friction force between tip and sample. Already small viscous damping contributions in the tip–sample contact are sufficient to suppress stick–slip oscillations.     

开放式多功能扫描探针显微镜系统

开放式多功能扫描探针显微镜、集成扫描隧道显微镜、原子力显微镜、横向力显微镜和静电力显微镜．具有接触、半接触和非接触工作模式，可进行作用力、电流、电位、光能量等参数的高度局域综合测量,具有极高的开放性和可扩展性，支持用户进行二次开发。     

Theoretical comparison of illumination and collection mode images of magneto-optical dots

We compare theoretical images of the same sample obtained with two different scanning near-field optical microscopes. The sample is a two-dimensional periodic array of magnetic sub-micrometric dots. The magnetization is perpendicular to the sample plane (polar magnetization). The first configuration is a scanning tunnelling optical near-field microscope (STOM) where the tip is used in the detection mode and the sample is illuminated by total internal reflection. The second configuration is an inverted STOM: the tip is used in the emission mode and the diffracted field is far-field detected in one direction. We present the models used to describe the two configurations and then explain the main lines of the formalism used to calculate the diffracted fields by a magneto-optical sample.     

Characterization of the cutting edge of glass knives for ultramicrotomy by scanning force microscopy using cantilevers with a defined tip geometry

The geometry of glass knife edges for ultramicrotomy was studied with nanoscale resolution using scanning force microscopy (SFM) in the contact mode. The local shape of the cutting edge was estimated from single line profiles of the SFM topographic images by taking into account the exact radius of the ultrasharp silicon tip. The tip radius was estimated from secondary electron micrographs recorded at low voltage by field emission scanning electron microscopy (FESEM). The radius of the investigated cutting edges was found to be in range 5–20 nm. The results obtained illustrate that the combination of SFM and high resolution FESEM provides a unique means to determine precisely the radius of glass knives.     

Multifrequency high-speed phase-modulation atomic force microscopy in liquids

We have developed a new technique, called multifrequency high-speed phase-modulation atomic force microscopy (PM-AFM) in constant-amplitude (CA) mode based on the simultaneous excitation of the first two flexural modes of a cantilever. By performing a theoretical investigation, we have found that this technique enables the simultaneous imaging of the surface topography, energy dissipation and elasticity (nonlinear mapping) of materials. We experimentally demonstrated high-speed imaging at a scan speed of 5 frames/s for a polystyrene (PS) and polyisobutylene (PIB) polymer-blend thin-film surface in water.     

Effects of tip-sample forces and humidity on the imaging of DNA with a scanning force microscope

We have investigated the effects of tip-sample forces and relative humidity when using a scanning force microscope (SFM) to image DNA molecules adsorbed on fresh mica. As the force between the tip and the sample increases, the apparent height of the DNA molecules decreases. After being imaged with high forces, the DNA molecules recover partially in their apparent height, indicating that a plastic deformation of the DNA has been induced by the scanning tip. At low humidities, DNA molecules can be imaged with a force up to 150 nN during the scanning without obvious damages. At higher humidities, however, the DNA molecules can be dissected or swept away by the tip even at a tip-sample force of 30 nN. The net force between the tip and the molecules is the vector sum of several forces, the dominant components of which are the elastic force due to the cantilever bending and the capillary force resulting from the water meniscus formed between the tip and the sample surface. When the relative humidity of the imaging environment is increased, the capillary force becomes stronger.     

Scanning probe microscopy for industrial applications: Selected examples

Some examples are selected to demonstrate the variety of possible scanning probe microscopy application in industry. Magnetic and magneto-optical storage media can be investigated by magnetic force microscopy, whereas a conventional scanning force microscope is used to examine surface features of many different materials, such as technical glasses, photosensitive materials, new superconductors, and biomolecules. Some other examples include the modification as well as the observation of liquid crystal devices, and the impact that scanning probe microscopy has on other techniques such as high precision stepping motors and high quality electron beam sources.