Time of flight grazing incidence small angle neutron scattering

Grazing incidence small angle neutron scattering (GISANS) overcomes the limitations of conventional small angle scattering with respect to extremely small sample volumes in the thin film geometry. In time of flight (TOF) mode neutrons with a broad range of wavelengths are used simultaneously and recorded as a function of their respective times of flight. The combination of both, TOF-GISANS, enables the simultaneous performance of several GISANS measurements, which differ in wavelength. As a consequence, within one measurement a full set of GISANS pattern related to different scattering vectors, different scattering depths and resolutions result. This allows the detection of nanostructures with a chemical sensitivity. The possibilities of TOF-GISANS are demonstrated by the simple example of polymer nano-dots located on top of a silicon surface. As probed with atomic force microscopy (AFM) the nano-dots exhibit a large characteristic nearest neighbour distance of 545 nm and a surface coverage of 28%. From the analysis of the wavelength dependent data in combination with AFM the mass density of the polymer nano-dots is determined to be equal to the bulk value. A comparison to common single wavelength GISANS experiments is shown.     

Nano- and micro-scale patterning of Si (1 0 0) under keV ion irradiation

Evolution of Si (1 0 0) surface under 100 keV Ar⁺ ion irradiation at oblique incidence has been studied. The dynamics of surface erosion by ion beam is investigated using detailed analysis of atomic force microscopy (AFM) measurements. During an early stage of sputtering, formation of almost uniformly distributed nano-dots occurs on Si surface. However, the late stage morphology is characterized by self-organization of surface into a regular ripple pattern. Existing theories of ripple formation have been invoked to provide an insight into surface rippling.     

水溶液中PbS纳米晶生长过程的原位光谱检测

为了研究纳米晶在溶液中的生长规律,设计并实现了一个能够实时监测纳米晶生长的原位透射光谱系统。利用该系统对PbS纳米线和纳米点在水相中生长过程进行了原位光谱检测,发现十二烷基硫酸钠对PbS纳米晶的定向生长起了非常重要的作用。     

高速率沉积磁控溅射技术制备Ge点的退火生长研究

采用磁控溅射技术在Si衬底上以350?C沉积14 nm的非晶Ge薄膜,通过退火改变系统生长热能,实现了低维Ge/Si点的生长.利用原子力显微镜(AFM)和拉曼(Raman)光谱所获得的形貌和声子振动信息,对Ge点的形成机理和演变规律进行了研究.实验结果表明:在675?C退火30 min后,非晶Ge薄膜转变为密度高达8.5×109cm-2的Ge点.通过Ostwald熟化理论、表面扩散模型和对激活能的计算,很好地解释了退火过程中,Ge原子在Si表面迁移、最终形成纳米点的行为.研究结果表明用高速沉积磁控溅射配合热退火制备Ge/Si纳米点的方法,可为自组织量子点生长实验提供一定的理论支撑.     

Pinning potential in thick PrBa2Cu3Ox/YBa2Cu3O7−δ quasi-multilayers

Using Pulsed Laser Deposition we have fabricated thick quasi-multilayers composed of incomplete layers of PrBa₂Cu₃O_x (PrBCO) nano-dots and layers of YBa₂Cu₃O_7?δ (YBCO). The number of such sequences was between 2 and 6, with the thickness of individual YBCO layers between 565 and 885 nm, and total thickness between 1.13 and 5.31 μm. For the thinner quasi-multilayer, DC magnetization studies showed an increase in the critical current density J_c at all fields in comparison with a pure YBCO reference sample, while the thicker samples showed an increased J_c only in high fields. We have also investigated the frequency dependence of J_c from AC susceptibility studies and found that the pinning potential is well described by a logarithmic dependence on current density. Pinning potentials in PrBCO/YBCO quasi-multilayers also proved to be higher than in the reference sample at high fields. From angle-dependent transport measurements we have found indications of strong pinning centres induced by the (PrBCO) nano-dots, both isotropic and c-axis correlated.     

Understanding tapping-mode atomic force microscopy data on the surface of soft block copolymers

In this paper, we focus on better understanding tapping-mode atomic force microscopy (AFM) data of soft block copolymer materials with regard to: (1) phase attribution; (2) the relationship between topography and inside structure; (3) contrast-reversal artifacts; (4) the influence of annealing treatment on topography. The experiments were performed on the surface of poly(styrene–ethylene/butylene–styrene) (SEBS) triblock copolymer acting as a model system. First, by coupling AFM with transmission electron microscopy (TEM) measurements, the phase attribution for AFM images was determined. Secondly, by imaging an atomically flat SEBS surface as well as an AFM tip-scratched SEBS surface, it was confirmed that the contrast in AFM height images of soft block copolymers is not necessarily the result of surface topography but the result of lateral differences in tip-indentation depth between soft and hard microdomains. It was also found that there is an enlarging effect in AFM images on the domain size of block copolymers due to the tip-indention mechanism. Thirdly, based on the tip-indention mechanism, tentative explanations in some detail for the observed AFM artifacts (a reversal in phase image followed by another reversal in height image) as function of imaging parameters were given. Last, it was demonstrated that the commonly used annealing treatments in AFM sample preparation of block copolymers may in some cases lead to a dramatic topography change due to the unexpected order-to-order structure transition.     

Position-controlled marker formation by helium ion microscope for aligning a TEM tomographic tilt series

We formed nano-dots using a helium ion microscope (HIM) equipped with a gas injection system. Because of position controllability, the nano-dot markers could be placed efficiently on a specimen using the HIM. The sizes of the dots were controlled by changing the beam radiation time. We tried for the first time to form dots on a rod-shaped specimen to use them as markers for aligning a transmission electron microscope tomographic tilt series before reconstructing 3D images.     

AFM tip gauge by nuclear tracks methodology

Atomic force microscopy (AFM) instrumentation in the different modes of operation is a metrologic system for evaluating some surface properties of solid and semisolid materials. The resolution of this instrument depends strongly on the tip sharpness, which can be changed by contamination of the AFM tip apex due to wearing and/or breaking. In order to assess new and old tips, scanning electron microscopy (SEM) inspection is often used, which is not very convenient due to the availability and demand of SEM services. In the market there are some expensive devices for verification of the tip geometry, and for the particular case of AFM in the tapping mode, a simple proposal has been published based on fiber-like samples. In this work, we present an AFM tip gauge device based on the use of a pattern of etched tracks on CR-39 material. For the preparation of the device, the requirements are a radioactive alpha particle source with specific energy, controlled temperature bath and KOH solution, with all these parameters optimized for the tip evaluation, based on the AFM profilometry image. This work shows another interesting and a very useful application of nuclear tracks methodology (NTM).     

Observations of fission-tracks in zircons by atomic force microscope

The fission-track (FT) method is a dating technique based on the observation of damage (tracks) by spontaneous fission of ²³⁸U left in a mineral. The date is calculated from the track density and the uranium concentration in the mineral. This is possible because the number of tracks is a function of uranium concentration and time since the start of track accumulation. Usually, the number of tracks is counted under an optical microscope after etching (chemical expansion of a track). However, as FT density per unit area rises, it becomes difficult to count the number of tracks. This is due to the fact that FTs overlap one another and are unable to be readily distinguished. This research examines the potential of atomic force microscope (AFM) for FT dating using zircons, which are likely to show higher FT density than other minerals due to their high U concentrations.To obtain an AFM image for a sample prepared for FT dating, removing the static electricity of the sample is essential to avoid an unexpected movement of the cantilever. A grain should be wider than about 30 μm to bring the cantilever on the mineral surface. Polishing with a fine grained compound is very important. There is not much difference in sharpness between images by AC mode (scanning with vibrating cantilever at a constant cycle) and Contact mode (scanning with the cantilever always in close contact with the surface). To confirm how tracks can be identified with the AFM, an AFM image was compared with an image obtained with the optical microscope. When change in the number of tracks and their shapes were observed through stepwise etching, the track expanded as the etching time increased. In addition, the etching rate was slower for large tracks than those for small tracks. This implied that the AFM can be used to observe etching of zircons with different degrees of nuclear fission damage. A track that could not be seen with the optical microscope due to insufficient etching could be observed by AFM methods, indicating the possibility of FT dating with high track densities using AFM after relatively short etching periods.     

Surface defects characterization with frequency and force modulation atomic force microscopy using molecular dynamics simulations

This paper is devoted to the characterization of the surface defects using a recently developed AFM technique called frequency and force modulation AFM (FFM–AFM). The simulated system includes a recently developed gold coated AFM probe which interacts with a sample including single-atom vacancy and impurities. In order to examine the behavior of the above system on different transition metals, the molecular dynamics (MD) simulation with Sutton–Chen (SC) inter-atomic potential is used. In this study, an online imaging simulation of the probe and sample is performed, and the effects of the horizontal scan speed, the effective frequency set-point, the cantilever stiffness, the tip-sample rest position and the cantilever quality factor on the resulting images are investigated. Using a proposed optimum controlling scheme for the excitation force amplitude, the cantilever horizontal speed can be increased.     

Charged vortex structure in high-temperature superconductors

By using a model Hamiltonian with competing antiferromagnetic (AFM) spin density wave (SDW) and d-wave superconductivity orders, the effect of next-nearest-neighbour (nnn) hopping on spin and charge structures in high-temperature superconductors is investigated at finite temperatures. For an optimally doped sample, we find that the AFM order magnitude in the vortex core is firstly enhanced and then suppressed, accompanied with a ``positively → negatively → positively" charged vortex structure transition with increasing nnn hopping strength, which implies that the AFM order is unnecessarily bounded to an electron-rich vortex core. In addition, a charge ordering pattern with four negatively charged peaks localized in a small region is also found around the vortex core centre without net charge. Recent scanning-tunneling-microscopy experimental observations of the checkerboard structure are hopefully understood.     

The size dependence of the nano-dots formed by electron-beam-induced deposition on the partial pressure of the precursor

We have successfully fabricated nano-dots containing W from a metal–organic gas source by electron-beam-induced deposition in an ultra-high vacuum transmission electron microscope. The size of the dots can be controlled by changing the time for irradiation and the partial pressure of the precursor. The smallest particle size is less than 2 nm in diameter, which is the record smallest ever made by this method. PACS 68.37.Lp; 81.07.-b; 81.16.-c     

Numerical study of the hydrodynamic drag force in atomic force microscopy measurements undertaken in fluids

When atomic force microscopy (AFM) is employed for in vivo study of immersed biological samples, the fluid medium presents additional complexities, not least of which is the hydrodynamic drag force due to viscous friction of the cantilever with the liquid. This force should be considered when interpreting experimental results and any calculated material properties. In this paper, a numerical model is presented to study the influence of the drag force on experimental data obtained from AFM measurements using computational fluid dynamics (CFD) simulation. The model provides quantification of the drag force in AFM measurements of soft specimens in fluids.The numerical predictions were compared with experimental data obtained using AFM with a V-shaped cantilever fitted with a pyramidal tip. Tip velocities ranging from 1.05 to 105 μm/s were employed in water, polyethylene glycol and glycerol with the platform approaching from a distance of 6000 nm. The model was also compared with an existing analytical model. Good agreement was observed between numerical results, experiments and analytical predictions. Accurate predictions were obtained without the need for extrapolation of experimental data. In addition, the model can be employed over the range of tip geometries and velocities typically utilized in AFM measurements.     

Surface modification of γ-TiAl alloys by acetylene plasma deposition

Surfaces of two γ-TiAl alloys, Ti-47 at% Al-2at% Nb-2 at% Cr (MJ12) and Ti-47 at% Al-2 at% Nb-2 at% Mn + 0.8 at% TiB₂ (MJ47), have been modified by acetylene plasma deposition at bias voltages of −4, −5 and −6 kV for 3.6 × 10³ s (1 h) and 1.44 × 10⁴ s (4 h). Knoop hardness (HK) of the alloys is increased with the increase of bias voltage and prolonged time for the deposition. HK of MJ12 and MJ47 deposited at −6 kV for 1.44 × 10⁴ s is, respectively, 3.36 and 3.32 times as hard as the untreated alloys. SEM and AFM analyses show that the deposited alloys compose of a number of nano-dots which reflect their surface properties. The phases analyzed by XRD are in accord with the elements analyzed by EDX.     

Selective growth of stacked InAs quantum dots by using the templates formed by the Nano-Jet Probe

We have demonstrated the selective area growth of stacked self-assembled InAs quantum dot (QD) arrays in the desired regions on a substrate and confirmed the photoluminescence (PL) emission exhibited by them at room temperature. These InAs QDs are fabricated by the use of a specially designed atomic force microscope cantilever referred to as the Nano-Jet Probe (NJP). By using the NJP, two-dimensional arrays with ordered In nano-dots are fabricated in the desired square regions on a GaAs substrate and directly converted into InAs QD arrays through the subsequent annealing by the irradiation of As flux. By using the converted QD arrays as strain templates, self-organized InAs QDs are stacked. These stacked QDs exhibit the PL emission peak at a wavelength of 1.02 μm.     

The magnetoresistive effect induced by stress in spin-valve structure

Using a method of free energy minimization, this paper investigates the magnetization properties of a ferromagnetic (FM) monolayer and an FM/antiferromagnetic (AFM) bilayer under a stress field, respectively. It then investigates the magnetoresistance (MR) of the spin-valve structure, which is built by an FM monolayer and an FM/AFM bilayer, and its dependence upon the applied stress field. The results show that under the stress field, the magnetization properties of the FM monolayer is obviously different from that of the FM/AFM bilayer, since the coupled AFM layer can obviously block the magnetization of the FM layer. This phenomenon makes the MR of the spin-valve structure become obvious. In detail, there are two behaviors for the MR of the spin-valve structure dependence upon the stress field distinguished by the coupling (FM coupling or AFM coupling) between the FM layer and the FM/AFM bilayer. Either behavior of the MR of the spin-valve structure depends on the stress field including its value and orientation. Based on these investigations, a perfect mechanical sensor at the nano-scale is suggested to be devised experimentally.     

Effect of ultrasonic treatment on the morphology of casein particles

In this study, the effect of ultrasonic treatment duration on the morphology of self-assembled casein particles was investigated by atomic force microscopy (AFM), low vacuum scanning electron microscopy (SEM) and transmission electron microscopy (TEM). In the case of AFM images, the particle analysis which was carried out by the SPIP program showed that the self-assembled casein particles after being ultrasonically treated for 2 min got smaller in size compared to the casein particles that have not been exposed to any ultrasonic treatment. Surprisingly, however, increasing the ultrasonic time exposure of the particles resulted in an opposite effect where larger particles or aggregates seemed to be present. We show that by comparing the results obtained by AFM, SEM and TEM, the information extracted from the AFM images and analyzed by SPIP program give more detailed insights into particle sizes and morphology at the molecular level compared to SEM and TEM images, respectively.     

Water-solid interfaces probed by high-resolution atomic force microscopy

Water-solid interfaces play important roles across a broad range of scientific and application fields. In the past decades, atomic force microscopy (AFM) has significantly deepened our understanding of water-solid interfaces at molecular scale. In this review, we describe the recent progresses on probing water-solid interfaces by noncontact AFM, highlighting the imaging of interfacial water with ultrahigh spatial resolution. In particular, the recent development of qPlus-based AFM with functionalized tips has made it possible to directly image the H-bonding skeleton of interfacial water under UHV environment. Based on high-order electrostatic forces, such a technique even enables submolecular-level imaging of weakly bonded water structures with negligible disturbance. In addition, the three-dimensional (3D) AFM using low-noise cantilever deflection sensors can achieve atomic resolution imaging at liquid/solid interfaces, which opens up the possibility of probing the hydration layer structures under realistic conditions. We then discuss the application of those AFM techniques to various interfacial water systems, including water clusters, ion hydrates, water chains, water monolayers/multilayers and bulk water/ice on different surfaces under UHV or ambient environments. Some important issues will be addressed, including the H-bonding topology, ice nucleation and growth, ion hydration and transport, dielectric properties of water, etc. In the end, we present an outlook on the directions of future AFM studies of water at interfaces and the challenges faced by this field, as well as the development of new AFM techniques.     

Exchange-coupling-induced fourfold magnetic anisotropy in CoFeB/FeRh bilayer grown on SrTiO3(001)

Exchange coupling across the interface between a ferromagnetic (FM) layer and an antiferromagnetic (AFM) or another FM layer may induce a unidirectional magnetic anisotropy and/or a uniaxial magnetic anisotropy, which has been extensively studied due to the important application in magnetic materials and devices. In this work, we observed a fourfold magnetic anisotropy in amorphous CoFeB layer when exchange coupling to an adjacent FeRh layer which is epitaxially grown on an SrTiO₃(001) substrate. As the temperature rises from 300 K to 400 K, FeRh film undergoes a phase transition from AFM to FM phase, the induced fourfold magnetic anisotropy in the CoFeB layer switches the orientation from the FeRh$\langle 110\rangle $ to FeRh$\langle 100\rangle $ directions and the strength is obviously reduced. In addition, the effective magnetic damping as well as the two-magnon scattering of the CoFeB/FeRh bilayer also remarkably increase with the occurrence of magnetic phase transition of FeRh. No exchange bias is observed in the bilayer even when FeRh is in the nominal AFM state, which is probably because the residual FM FeRh moments located at the interface can well separate the exchange coupling between the below pinned FeRh moments and the CoFeB moments.     

Peculiarities of stochastic motion in antiferromagnetic nanoparticles

Antiferromagnetic (AFM) materials are widely used in spintronic devices as passive elements (for stabilization of ferromagnetic layers) and as active elements (for information coding). In both cases the switching between different AFM states, to a great extent depends on the environmental noise. In the present paper we derive stochastic Langevian equations for an AFM vector and a corresponding Fokker-Plank equation for a distribution function in the phase space of generalised coordinate and momentum. Thermal noise is modelled by a random delta-correlated magnetic field that interacts with the dynamic magnetisation of AFM particle. We scrupulously analyse a particular case of a collinear compensated AFM in the presence of spin-polarised current. The energy distribution function is found for normal modes in the vicinity of two equilibrium states (static and stationary) in sub- and super-critical regimes. It is shown that the noise-induced dynamics of AFM vector has some pecuilarities compared to the dynamics of magnetisation vector in ferromagnets.