Crystalline defect analysis in epitaxial Si0.7Ge0.3 layer using site-specific ECCI-STEM.

Electron channeling contrast imaging (ECCI) is a powerful technique to characterize the structural defects present in a sample and to obtain relevant statistics about their density. Using ECCI, such defects can only be properly visualized, if the information depth is larger than the depth at which defects reside. Furthermore, a systematic correlation of the features observed by ECCI with the defect nature, confirmed by a complementary technique, is required for defect analysis. Therefore, we present in this paper a site-specific ECCI-scanning transmission electron microscopy (STEM) inspection. Its value is illustrated by the application to a partially relaxed epitaxial Si0.7Ge0.3 on a Si substrate. All experiments including the acquisition of ECCI micrographs, the carbon marking and STEM specimen preparation by focused ion beam, and the in-situ-subsequent-STEM-in-scanning electron microscopy (SEM) characterization were executed in one SEM/FIB-based system, thus significantly improving the analysis efficiency. The ECCI information depth in Si0.7Ge0.3 has been determined through measuring stacking fault widths using different beam energies. ECCI is further utilized to localize the defects for STEM sample preparation and in-situ-subsequent-STEM-in-SEM investigation. This method provides a correlative 2.5D defect analysis from both the surface and cross-section. Using these techniques, the nature of different line-featured defects in epilayers can be classified, as illustrated by our study on Si0.7Ge0.3, which helps to better understand the formation of those detrimental defects.

Tuneable in-situ nanoCT workflow using FIB/SEM.

Inspired by the standard computed tomography, a new method of 3D X-ray imaging embedded in FIB-SEM microscope is proposed. The unique combination of TEM-like specimen stage enabling in lens STEM detection (referred to as CompuStage), nanomanipulator (referred to as EasyLift) facilitating in-situ sample transfer from bulk sample to TEM-like stage and pixelated in-situ Timepix X-ray detector in Helios G4 FX FIB-SEM system offers an unprecedented workflow. Motivated by common circular CT scan known from microCT world, the object under study is placed on CompuStage rod which enables two possible rotation (in TEM/SEM terminology called tilt) movements - α-tilt - rotation of the CompuStage rod around its axis, and ß-tilt - rotation around axis perpendicular to CompuStage rod. ß-tilt rotation enables a circular movement of the sample while α-tilt sets the correct position of sample with respect to target and detector. Thin metal lamella of suitable material welded to EasyLift manipulator needle is used as an X-ray target. The final target-sample geometry - position, distance - can be fine-tuned using position control of CompuStage and EasyLift and in-situ monitored by SEM. Both sample and target can also be easily prepared in-situ. Radiographs are recorded by Timepix detector with inherent noise-free operation and energy filtration. For the 3D reconstruction standard microCT reconstruction algorithm is used with the procedure adjusted for the format and quality of nanoCT images. The experiments were carried out on Helios G4 FX DualBeam using titanium and tungsten targets and various semiconductor samples. The ultimate resolution of the proposed method in orders of tens of nanometers was achieved both by the possibility of close target to sample positioning and of adjustment of primary beam energy down to low energies reducing the interaction volume in the target. Since the lower energy radiation is well suited for life-science, the method was also tested on several bio-samples using silver target. The silver target, thanks to its massive low energy Lα line, allowed to distinguish subtle structures in the resin embedded stained mouse brain and also to observe and reconstruct canaliculi in the mouse bone (earlier reported by Dierolf et al. 2010, Nature 467 436).

Application of electron channeling contrast imaging to 3D semiconductor structures through proper detector configurations.

Nowadays electron channeling contrast imaging (ECCI) is widely used to characterize crystalline defects on blanket semiconductors. Its further application in the semiconductor industry is however challenged by the emerging rise of nanoscale 3D heterostructures. In this study, an angular multi-segment detector is utilized in backscatter geometry to investigate the application of ECCI to the defect analysis of 3D semiconductor structures such as III/V nano-ridges. We show that a low beam energy of 5 keV is more favorable and that the dimension of 3D structures characterized by ECCI can be scaled down to ~ 28 nm. Furthermore, the impact of device edges on the collected ECCI image is investigated and correlated with tool parameters and cross-section profiles of the 3D structures. It is found that backscattered electrons (BSE) emitted from the device edge sidewalls and generating the bright edges (edge effects), share a similar angular distribution to those emitted from the surface. We show that the collection of low angle BSEs can suppressed the edge effects, however, at the cost of losing the defect contrast. A positive stage bias suppresses edge effects by removing the inelastically backscattered electrons from the sidewalls, but low loss BSEs from the sidewalls still contribute to the ECCI micrographs. On the other hand, if segments of an angular backscatter (ABS) detector are properly aligned with the nano-ridges, BSEs emitted from the sidewall and the surface can be separated, thus leading to the completely absence of one bright edge on the surface without compromise of the defect contrast. The merging of two such ECCI images reveals the nano-ridge surface without edge effects.

Enhancing the defect contrast in ECCI through angular filtering of BSEs.

In this study, an annular multi-segment backscattered electron (BSE) detector is used in back scatter geometry to investigate the influence of the angular distribution of BSE on the crystalline defect contrast in electron channeling contrast imaging (ECCI). The study is carried out on GaAs and Ge layers epitaxially grown on top of silicon (Si) substrates, respectively. The influence of the BSE detection angle and landing energy are studied to identify the optimal ECCI conditions. It is demonstrated that the angular selection of BSEs exhibits strong effects on defect contrast formation with variation of beam energies. In our study, maximum defect contrast can be obtained at BSE detection angles 53-65° for the investigated energies 5, 10 and 20 keV. In addition, it is found that higher beam energy is favorable to reveal defects with stronger contrast whereas lower energy ( ≤ 5 keV) is favorable for revealing crystalline defects as well as with topographic features on the surface. Our study provides optimal ECCI conditions, and therefore enables a precise and fast detection of threading dislocations in lowly defective materials and nanoscale 3D semiconductor structures where signal to noise ratio is especially important. A comparison of ECCI with BSE and secondary electron imaging further demonstrates the strength of ECCI in term of simultaneous detection of defects and morphology features such as terraces with atomic step heights.

Non-destructive characterization of extended crystalline defects in confined semiconductor device structures.

Semiconductor heterostructures are at the heart of most nanoelectronic and photonic devices such as advanced transistors, lasers, light emitting diodes, optical modulators and photo-detectors. However, the performance and reliability of the respective devices are often limited by the presence of crystalline defects which arise from plastic relaxation of misfit strain present in these heterogeneous systems. To date, characterizing the nature and distribution of such defects in 3D nanoscale devices precisely and non-destructively remains a critical metrology challenge. In this paper we demonstrate that electron channeling contrast imaging (ECCI) is capable of analyzing individual dislocations and stacking faults in confined 3D nanostructures, thereby fulfilling the aforementioned requirements. For this purpose we imaged the intensity of electrons backscattered from the sample under test under controlled diffraction conditions using a scanning electron microscope (SEM). In contrast to transmission electron microscopy (TEM) analysis, no electron transparent specimens need to be prepared. This enables a significant reduction of the detection limit (i.e. lowest defect density that can be assessed) as our approach facilitates the analysis of large sampling volumes, thereby providing excellent statistics. We applied the methodology to SiGe nanostructures grown by selective area epitaxy to study in detail how the nature and distribution of crystalline defects are affected by the dimensions of the structure. By comparing our observations with the results obtained using X-ray diffraction, TEM and chemical defect etching, we could verify the validity of the method. Our findings firmly establish that ECCI must be considered the method of choice for analyzing the crystalline quality of 3D semiconductor heterostructures with excellent precision even at low defect densities. As such, the technique aids in better understanding of strain relaxation and defect formation mechanisms at the nanoscale and, moreover, facilitates the development and fabrication of next generation nanoelectronic and photonic devices.

The Synergic Effect of Atomic Hydrogen Adsorption and Catalyst Spreading on Ge Nanowire Growth Orientation and Kinking.

Hydride precursors are commonly used for semiconductor nanowire growth from the vapor phase and hydrogen is quite often used as a carrier gas. Here, we used in situ scanning electron microscopy and spatially resolved Auger spectroscopy to reveal the essential role of atomic hydrogen in determining the growth direction of Ge nanowires with an Au catalyst. With hydrogen passivating nanowire sidewalls the formation of inclined facets is suppressed, which stabilizes the growth in the ⟨111⟩ direction. By contrast, without hydrogen gold diffuses out of the catalyst and decorates the nanowire sidewalls, which strongly affects the surface free energy of the system and results in the ⟨110⟩ oriented growth. The experiments with intentional nanowire kinking reveal the existence of an energetic barrier, which originates from the kinetic force needed to drive the droplet out of its optimum configuration on top of a nanowire. Our results stress the role of the catalyst material and surface chemistry in determining the nanowire growth direction and provide additional insights into a kinking mechanism, thus allowing to inhibit or to intentionally initiate spontaneous kinking.

Toward site-specific dopant contrast in scanning electron microscopy.

Since semiconductor devices are being scaled down to dimensions of several nanometers there is a growing need for techniques capable of quantitative analysis of dopant concentrations at the nanometer scale in all three dimensions. Imaging dopant contrast by scanning electron microscopy (SEM) is a very promising method, but many unresolved issues hinder its routine application for device analysis, especially in cases of buried layers where site-specific sample preparation is challenging. Here, we report on optimization of site-specific sample preparation by the focused Ga ion beam (FIB) technique that provides improved dopant contrast in SEM. Similar to FIB lamella preparation for transmission electron microscopy, a polishing sequence with decreasing ion energy is necessary to minimize the thickness of the electronically dead layer. We have achieved contrast values comparable to the cleaved sample, being able to detect dopant concentrations down to 1×10(16) cm-3. A theoretical model shows that the electronically dead layer corresponds to an amorphized Si layer formed during ion beam polishing. Our results also demonstrate that contamination issues are significantly suppressed for FIB-treated samples compared with cleaved ones.

Real-time observation of collector droplet oscillations during growth of straight nanowires.

A liquid droplet sitting on top of a pillar is crucially important for semiconductor nanowire growth via a vapor-liquid-solid (VLS) mechanism. For the growth of long and straight nanowires, it has been assumed so far that the droplet is pinned to the nanowire top and any instability in the droplet position leads to nanowire kinking. Here, using real-time in situ scanning electron microscopy during germanium nanowire growth, we show that the increase or decrease in the droplet wetting angle and subsequent droplet unpinning from the growth interface may also result in the growth of straight nanowires. Because our argumentation is based on terms and parameters common for VLS-grown nanowires, such as the geometry of the droplet and the growth interface, these conclusions are likely to be relevant to other nanowire systems.

Guided assembly of gold colloidal nanoparticles on silicon substrates prepatterned by charged particle beams.

Colloidal gold nanoparticles represent technological building blocks which are easy to fabricate while keeping full control of their shape and dimensions. Here, we report on a simple two-step maskless process to assemble gold nanoparticles from a water colloidal solution at specific sites of a silicon surface. First, the silicon substrate covered by native oxide is exposed to a charged particle beam (ions or electrons) and then immersed in a HF-modified solution of colloidal nanoparticles. The irradiation of the native oxide layer by a low-fluence charged particle beam causes changes in the type of surface-terminating groups, while the large fluences induce even more profound modification of surface composition. Hence, by a proper selection of the initial substrate termination, solution pH, and beam fluence, either positive or negative deposition of the colloidal nanoparticles can be achieved.

Low energy focused ion beam milling of silicon and germanium nanostructures.

In this paper focused ion beam milling of very shallow nanostructures in silicon and germanium by low energy Ga( + ) ions is studied with respect to ion beam and scanning parameters. It has been found that, using low energy ions, many scanning artefacts can be avoided and, additionally, some physical effects (e.g. redeposition and ion channelling) are significantly suppressed. The structures milled with low energy ions suffer less subsurface ion beam damage (amorphization, formation of voids) and are thus more suitable for selected applications in nanotechnology.

Ultrasoft magnetic films investigated with Lorentz tranmission electron microscopy and electron holography.

As a tribute to the scientific work of Professor Gareth Thomas in the field of structure-property relationships this paper delineates a new possibility of Lorentz transmission electron microscopy (LTEM) to study the magnetic properties of soft magnetic films. We show that in contrast to the traditional point of view, not only does the direction of the magnetization vector in nano-crystalline films make a correlated small-angle wiggling, but also the magnitude of the magnetization modulus fluctuates. This fluctuation produces a rapid modulation in the LTEM image. A novel analysis of the ripple structure in nano-crystalline Fe-Zr-N film corresponds to an amplitude of the transversal component of the magnetization deltaMy of 23 mT and a longitudinal fluctuation of the magnetization of the order of deltaMx = 30 mT. The nano-crystalline (Fe99Zr1)1-xNx films have been prepared by DC magnetron reactive sputtering with a thickness between 50 and 1000 nm. The grain size decreased monotonically with N content from typically 100 nm in the case of N-free films to less than 10 nm for films containing 8 at%. The specimens were examined with a JEOL 2010F 200 kV transmission electron microscope equipped with a post column energy filter (GIF 2000 Gatan Imaging Filter). For holography, the microscope is mounted with a biprism (JEOL biprism with a 0.6 microm diameter platinum wire).