Adeline Grenier

3D analysis of advanced nano-devices using electron and atom probe tomography.

The structural and chemical properties of advanced nano-devices with a three-dimensional (3D) architecture have been studied at the nanometre scale. An original method has been used to characterize gate-all-around and tri-gate silicon nanowire transistor by combining electron tomography and atom probe tomography (APT). Results show that electron tomography is a well suited method to determine the morphological structure and the dimension variations of devices provided that the atomic number contrast is sufficient but without an absolute chemical identification. APT can map the 3D chemical distribution of the atoms in devices but suffers from strong distortions in the dimensions of the reconstructed volume. These may be corrected using a simple method based on atomic density correction and electron tomography data. Moreover, this combination is particularly useful in helping to understand the evaporation mechanisms and improve APT reconstructions. This paper demonstrated that a full 3D characterization of nano-devices requires the combination of both tomography techniques.

Three dimensional imaging and analysis of a single nano-device at the ultimate scale using correlative microscopy techniques

The analysis of a same sample using nanometre or atomic-scale techniques is fundamental to fully understand device properties. This is especially true for the dopant distribution within last generation nano-transistors such as MOSFET or FINFETs. In this work, the spatial distribution of boron in a nano-transistor at the atomic scale has been investigated using a correlative approach combining electron and atom probe tomography. The distortions present in the reconstructed volume using atom probe tomography have been discussed by simulations of surface atoms using a cylindrical symmetry taking into account the evaporation fields. Electron tomography combined with correction of atomic density was used so that to correct image distortions observed in atom probe tomography reconstructions. These corrected atom probe tomography reconstructions then enable a detailed boron doping analysis of the device.

Self-adapting denoising, alignment and reconstruction in electron tomography in materials science

An automatic procedure for electron tomography is presented. This procedure is adapted for specimens that can be fashioned into a needle-shaped sample and has been evaluated on inorganic samples. It consists of self-adapting denoising, automatic and accurate alignment including detection and correction of tilt axis, and 3D reconstruction. We propose the exploitation of a large amount of information of an electron tomography acquisition to achieve robust and automatic mixed Poisson-Gaussian noise parameter estimation and denoising using undecimated wavelet transforms. The alignment is made by mixing three techniques, namely (i) cross-correlations between neighboring projections, (ii) common line algorithm to get a precise shift correction in the direction of the tilt axis and (iii) intermediate reconstructions to precisely determine the tilt axis and shift correction in the direction perpendicular to that axis. Mixing alignment techniques turns out to be very efficient and fast. Significant improvements are highlighted in both simulations and real data reconstructions of porous silicon in high angle annular dark field mode and agglomerated silver nanoparticles in incoherent bright field mode. 3D reconstructions obtained with minimal user-intervention present fewer artefacts and less noise, which permits easier and more reliable segmentation and quantitative analysis. After careful sample preparation and data acquisition, the denoising procedure, alignment and reconstruction can be achieved within an hour for a 3D volume of about a hundred million voxels, which is a step toward a more routine use of electron tomography.

Atomic arrangement at ZnTe/CdSe interfaces determined by high resolution scanning transmission electron microscopy and atom probe tomography

High resolution scanning transmission electron microscopy and atom probe tomography experiments reveal the presence of an intermediate layer at the interface between two binary compounds with no common atom, namely, ZnTe and CdSe for samples grown by Molecular Beam Epitaxy under standard conditions. This thin transition layer, of the order of 1 to 3 atomic planes, contains typically one monolayer of ZnSe. Even if it occurs at each interface, the direct interface, i.e., ZnTe on CdSe, is sharper than the reverse one, where the ZnSe layer is likely surrounded by alloyed layers. On the other hand, a CdTe-like interface was never observed. This interface knowledge is crucial to properly design superlattices for optoelectronic applications and to master band-gap engineering.

X-ray μ-Laue diffraction analysis of Cu through-silicon vias: A two-dimensional and three-dimensional study

Here, white X-ray μ-beam Laue diffraction is developed and applied to investigate elastic strain distributions in three-dimensional (3D) materials, more specifically, for the study of strain in Cu 10 μm diameter–80 μm deep through-silicon vias (TSVs). Two different approaches have been applied: (i) two-dimensional μ-Laue scanning and (ii) μ-beam Laue tomography. 2D μ-Laue scans provided the maps of the deviatoric strain tensor integrated along the via length over an array of TSVs in a 100 μm thick sample prepared by Focused Ion Beam. The μ-beam Laue tomography analysis enabled to obtain the 3D grain and elemental distribution of both Cu and Si. The position, size (about 3 μm), shape, and orientation of Cu grains were obtained. Radial profiles of the equivalent deviatoric strain around the TSVs have been derived through both approaches. The results from both methods are compared and discussed.

Quantitative investigation of SiGeC layers using atom probe tomography

The quantification of carbon and germanium in a Si/SiGeC multilayer structure using atom probe tomography has been investigated as a function of analysis conditions. The best conditions for quantitative results are obtained using an intermediate electric field and laser power. Carbon evaporation shows strong spatial and temporal correlation. By using multi-ion event analysis, an evaporation mechanism is put forward to explain the modification of mass spectra as a function of electric field and laser power.

Toward an accurate quantification in atom probe tomography reconstruction by correlative electron tomography approach on nanoporous materials

In this contribution, we propose a protocol for analysis and accurate reconstruction of nanoporous materials by atom probe tomography (APT). The existence of several holes in porous materials makes both the direct APT analysis and reconstruction almost inaccessible. In the past, a solution has been proposed by filling pores with electron beam-induced deposition. Here, we present an alternative solution using an electro-chemical method allowing to fill even small and dense pores, making APT analysis possible. Concerning the 3D reconstruction, the microstructural features observed by electron tomography are used to finely calibrate the APT reconstruction parameters.

Preparation and Analysis of Atom Probe Tips by Xenon Focused Ion Beam Milling.

The damage and ion distribution induced in Si by an inductively coupled plasma Xe focused ion beam was investigated by atom probe tomography. By using predefined patterns it was possible to prepare the atom probe tips with a sub 50 nm end radius in the ion beam microscope. The atom probe reconstruction shows good agreement with simulated implantation profiles and interplanar distances extracted from spatial distribution maps. The elemental profiles of O and C indicate co-implantation during the milling process. The presence of small disc-shaped Xe clusters are also found in the three-dimensional reconstruction. These are attributed to the presence of Xe nanocrystals or bubbles that open during the evaporation process. The expected accumulated dose points to a loss of >95% of the Xe during analysis, which escapes undetected.

Atomic Scale Structural Characterization of Epitaxial (Cd,Cr)Te Magnetic Semiconductor

A detailed knowledge of the atomic structure of magnetic semiconductors is crucial to understanding their electronic and magnetic properties, which could enable spintronic applications. Energy-dispersive X-ray spectrometry (EDX) in the scanning transmission electron microscope and atom probe tomography (APT) experiments reveal the formation of Cr-rich regions in Cd1-x Cr x Te layers grown by molecular beam epitaxy. These Cr-rich regions occur on a length scale of 6-10 nm at a nominal Cr composition of x=0.034 and evolve toward an ellipsoidal shape oriented along directions at a composition of x=0.083. Statistical analysis of the APT reconstructed volume reveals that the Cr aggregation increases with the average Cr composition. The correlation with the magnetic properties of such (Cd,Cr)Te layers is discussed within the framework of strongly inhomogeneous materials. Finally, difficulties in accurately quantifying the Cr distribution in the CdTe matrix on an atomic scale by EDX and APT are discussed.

Dopant radial inhomogeneity in Mg-doped GaN nanowires

Using atom probe tomography, it is demonstrated that Mg doping of GaN nanowires grown by Molecular Beam Epitaxy results in a marked radial inhomogeneity, namely a higher Mg content in the periphery of the nanowires. This spatial inhomogeneity is attributed to a preferential incorporation of Mg through the m-plane sidewalls of nanowires and is related to the formation of a Mg-rich surface which is stabilized by hydrogen. This is further supported by Raman spectroscopy experiments which give evidence of Mg-H complexes in the doped nanowires. A Mg doping mechanism such as this, specific to nanowires, may lead to higher levels of Mg doping than in layers, boosting the potential interest of nanowires for light emitting diode applications.