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A sample preparation method is described for enabling direct correlation of site-specific plan-view and cross-sectional transmission electron microscopy (TEM) analysis of individual nanostructures by employing a dual-beam focused-ion beam (FIB) microscope. This technique is demonstrated using Si nanowires dispersed on a TEM sample support (lacey carbon or Si-nitride). Individual nanowires are first imaged in the plan-view orientation to identify a region of interest; in this case, impurity atoms distributed at crystalline defects that require further investigation in the cross-sectional orientation. Subsequently, the region of interest is capped with a series of ex situ and in situ deposited layers to protect the nanowire and facilitate site-specific lift-out and cross-sectioning using a dual-beam FIB microscope. The lift-out specimen is thinned to electron transparency with site-specific positioning to within ∼200 nm of a target position along the length of the nanowire. Using the described technique, it is possible to produce correlated plan-view and cross-sectional view lattice-resolved TEM images that enable a quasi-3D analysis of crystalline defect structures in a specific nanowire. While the current study is focused on nanowires, the procedure described herein is general for any electron-transparent sample and is broadly applicable for many nanostructures, such as nanowires, nanoparticles, patterned thin films, and devices.
There is a wide array of technologically significant materials whose response to electric and magnetic fields can make or break their utility for specific applications. Often, these electrical and magnetic properties are determined by nanoscale features that can be most effectively understood through electron microscopy studies. Here, we present an overview of the capabilities for transmission electron microscopy for uncovering information about electric and magnetic properties of materials in the context of operational devices. When devices are operated during microscope observations, a wealth of information is available about dynamics, including metastable and transitional states. Additionally, because the imaging beam is electrically charged, it can directly capture information about the electric and magnetic fields in and around devices of interest. This is perhaps most relevant to the growing areas of nanomaterials and nanodevice research. Several specific examples are presented of materials systems that have been explored with these techniques. We also provide a view of the future directions for research.
One of the most widely studied types of magnetic nanostructure is that used in devices based on the giant magnetoresistance (GMR) or tunnel magnetoresistance (TMR) phenomena. In order to understand the behaviour of these materials it is important to be able to follow their magnetisation reversal mechanism, and one of the techniques enabling micromagnetic studies at the sub-micron scale is transmission electron microscopy. Two techniques can be used: Lorentz transmission electron microscopy and off-axis electron holography, both of which allow the magnetic domain structure of a ferromagnetic material to be investigated dynamically in real-time with a resolution of a few nanometres. These techniques have been used in combination with in situ magnetizing experiments, to carry out qualitative and quantitative studies of magnetization reversal in a range of materials including spin-tunnel junctions, patterned thin film elements and magnetic antidot arrays. Quantitative analysis of the Lorentz TEM data has been carried out using the transport of intensity equation (TIE) approach.
Extended abstract of a paper presented at the Pre-Meeting Congress: Materials Research in an Aberration-Free Environment, at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, July 31 and August 1, 2004.
The effect of the laser energy density used to deposit Bi onto amorphous aluminum oxide (a-Al2O3) on the growth of Bi nanocrystals has been investigated using transmission electron microscopy of cross section samples. The laser energy density on the Bi target was varied by one order of magnitude (0.4 to 5 J cm-2). Across the range of energy densities, in addition to the Bi nanocrystals nucleated on the a-Al2O3 surface, a dark and apparently continuous layer appears below the nanocrystals. Energy dispersive X-ray analysis on the layer have shown it is Bi rich. The separation from the Bi layer to the bottom of the nanocrystals on top is consistent with the implantation range of Bi species in a-Al2O3. As the laser energy density increases, the implantation range has been measured to increase. The early stages of the Bi growth have been analyzed in order to determine how the Bi implanted layer develops.
In recent years there has been a high degree of interest in multilayer film (MLF) structures because of their applications as magnetoresistive sensors and as memory elements in magnetoresistive random access memory arrays. As each of the layers in a spin-valve-based MLF structure1 is only a few nanometers in thickness, the morphology of the layers is crucial in controlling the magnetic and transport properties of the devices. In general, the microstructural features that can influence the film properties include layer roughness, layer composition, interfacial chemical mixing, grain size, grain boundary morphology, and crystallographic orientation, with the most important microstructural parameter being the nature of the interfaces between adjacent layers. With so many internal interfaces, each of which can have a different morphology and degree of intermixing, it is extremely difficult to determine the nature of each individual interface unless a technique is used that can analyze them independently, and with high spatial resolution.
Multilayer film (MLF) structures which exhibit giant-magnetoresistance (GMR) properties have applications in the areas of magnetic recording and computer memory. The magnetic properties of MLF structures are dependent upon structural and compositional variations at the atomic level. Thus, structural characterization with high spatial resolution, especially at layer interfaces, is important in order to optimize device performance with respect to processing and operating conditions. Atom probe field ion microscopy (APFIM) is one technique that has the capability to characterize the local structure and composition of MLF devices with sufficiently high resolution. However, a major difficulty has been successful specimen preparation from MLF materials, which requires fabrication of a sharply pointed needle (radius <50 nm) containing the layers of interest in the apex region. Research on specialized field ion specimen preparation techniques which use focused ion beam milling has recently enabled nanoscale MLF structures to be investigated. In the present paper, the application of atom probe microanalysis to two different MLF structures is presented.
Control and optimization of materials’ properties will increasingly depend on the ability to tailor both the structure and chemical composition of the materials at the nanoscale level (100 nm and less). One specific class of “nanostructured” materials is the multilayer film (MLF) structure, which is formed by alternate deposition of two or more different elements or compounds and has a wide range of applications in, for example, the field of data recording and storage. In order to understand MLF structures well enough to improve and optimize their properties, characterization at the atomic level with regard to both structure and chemistry is essential. Interface quality is one of the most important parameters due to the possibility of intermixing between layers. It is thus desirable to obtain information about the interface morphology in these materials at the highest possible resolution.
The Foucault and Fresnel modes of Lorentz microscopy, together with a
quantitative magnetization mapping technique, summed image differential
phase-contrast imaging, were used to study the magnetization reversal
mechanism of the sense layer in spin-valve structures exhibiting the giant
magnetoresistance effect. In addition to studies of sheet film,
lithographically defined spin-valve elements were investigated. A current
can be passed through the element during magnetizing so that the effect of
the applied current on the giant magnetoresistance and magnetization
reversal mechanism can be studied. Results are presented for a number of
different spin-valve structures.
Amorphous d.c. sputtered SbOx films (0.19< x<2.0) have been found to be fast crystallising materials sensitive to nano- and pico-second laser pulses, and have potential applications as optical data-storage media. They were crystallised in-situ in a JEOL 4000EX TEM, and the crystallisation recorded onto video tape. The crystallisation of the SbO0.37 films occurred by random nucleation followed by growth until coalescence. In contrast the crystallisation of the SbO0.533 films occurred by surface crystallisation across the whole film followed by bulk crystallisation through the film, during which contrast in the TEM increased steadily. Analysing the video frames in an image processing package enabled kinetic parameters such as transformation index and activation energy to be extracted. High resolution transmission electron microscopy showed the crystalline phase to contain nano-crystallites approximately 10 nm in size in a less-ordered matrix.
Atom-probe techniques have been used to characterise nanostructured metallic materials prepared by thermal evaporation and by sputtering. Multilayer samples of Fe-Cr have been prepared by sputter deposition and analysed using the Oxford position-sensitive atom probe. This has made it possible to observe the quality of interfaces in the material, and also accurately determine local compositions at each layer within the multilayer stack. Preliminary experiments aimed at producing dual phase nanocrystalline films by thermal evaporator deposition are also reported.
The atom probe field-ion microscope has been used to study the diffusion at interfaces in metallic multilayers deposited directly onto field-ion specimens and to develop models for the solid state reactions occuring at the atomic-scale in multilayer systems. Results are presented for the low temperature annealing of a Co-Ni multilayer. Intermixing over about 2 atomic planes is found even in as-deposited samples, extending to mnm after heating at 300°C for 1 hour. Using atom probe results from bulk alloys, a Monte Carlo simulation has been developed for the Fe-Cr system, in which a miscibility gap exists, and is being used in an attempt to model the behaviour of interfaces in Fe-Cr multilayers. Preliminary results are presented, showing that interfaces which are initially mixed over 10 atomic planes become sharper by an ‘interface spinodal’ reaction.