Atom-probe for FinFET dopant characterization

With the continuous shrinking of transistors and advent of new transistor architectures to keep in pace with Moore's law and ITRS goals, there is a rising interest in multigate 3D-devices like FinFETs where the channel is surrounded by gates on multiple surfaces. The performance of these devices depends on the dimensions and the spatial distribution of dopants in source/drain regions of the device. As a result there is a need for new metrology approach/technique to characterize quantitatively the dopant distribution in these devices with nanometer precision in 3D.In recent years, atom probe tomography (APT) has shown its ability to analyze semiconductor and thin insulator materials effectively with sub-nm resolution in 3D. In this paper we will discuss the methodology used to study FinFET-based structures using APT. Whereas challenges and solutions for sample preparation linked to the limited fin dimensions already have been reported before, we report here an approach to prepare fin structures for APT, which based on their processing history (trenches filled with Si) are in principle invisible in FIB and SEM. Hence alternative solutions in locating and positioning them on the APT-tip are presented. We also report on the use of the atom probe results on FinFETs to understand the role of different dopant implantation angles (10° and 45°) when attempting conformal doping of FinFETs and provide a quantitative comparison with alternative approaches such as 1D secondary ion mass spectrometry (SIMS) and theoretical model values.     

Complementary techniques for the characterization of thin film Ti/Nb multilayers

An aberration corrector on the probe-forming lens of a scanning TEM (STEM) equipped with an electron energy-loss spectrometer (EELS) and X-ray energy-dispersive spectrometer (XEDS) has been employed to investigate the compositional variations as a function of length scale in nanoscale Ti/Nb metallic multilayers. The composition profiles of EELS and XEDS were compared with the profiles obtained from the complementary technique of 3D atom probe tomography. At large layer widths (h≥7 nm, where h is the layer width) of Ti and Nb, XEDS composition profiles of Ti/Nb metallic multilayers are in good agreement with the EELS results. However, at reduced layer widths (h≈2 nm), profiles of EELS and atom probe exhibited similar compositional variations, whereas XEDS results have shown a marked difference. This difference in the composition profiling of the layers has been addressed with reference to the effects of beam broadening and the origin of the signals collected in these techniques. The advantage of using EELS over XEDS for these nanoscaled multilayered materials is demonstrated.     

Invited review article: Atom probe tomography

The technique of atom probe tomography (APT) is reviewed with an emphasis on illustrating what is possible with the technique both now and in the future. APT delivers the highest spatial resolution (sub-0.3-nm) three-dimensional compositional information of any microscopy technique. Recently, APT has changed dramatically with new hardware configurations that greatly simplify the technique and improve the rate of data acquisition. In addition, new methods have been developed to fabricate suitable specimens from new classes of materials. Applications of APT have expanded from structural metals and alloys to thin multilayer films on planar substrates, dielectric films, semiconducting structures and devices, and ceramic materials. This trend toward a broader range of materials and applications is likely to continue.     

Some aspects of the field evaporation behaviour of GaSb

In-depth analysis of pulsed laser atom probe tomography (APT) data on the field evaporation of the III-V semiconductor material GaSb reveals strong variations in charge states, relative abundances of different cluster ions, multiplicity of detector events and spatial correlation of evaporation events, as a function of the effective electric field at the specimen surface. These variations are discussed in comparison with the behaviour of two different metallic specimen materials, an Al-6XXX series alloy and pure W, studied under closely related experimental conditions in the same atom probe instrument. It is proposed that the complex behaviour of GaSb originates from a combination of spatially correlated evaporation events and the subsequent field induced dissociation of cluster ions, the latter contributing to inaccuracies in the overall atom probe composition determination for this material.     

Time evolution of morphology in mechanically alloyed Fe-Cu

Being widely accessible as well as already utilised in many applications, Fe-Cu acts as an ideal binary model alloy to elaborate the enforced nonequilibrium enhanced solubility in such a solution system that shows a limited regime of miscibility and characterised by a large positive heat of mixing. In addition to the detailed analysis of ball milled Fe-Cu powders by means of Atom Probe Tomography (APT), site specific structural analysis has been performed in this study using Transmission Electron Microscopy (TEM).In this contribution results on powders with low Cu concentrations (2.5-10 at%) are presented. Combining a ductile element (Cu, fcc) and a brittle one (Fe, bcc), striking differences in morphology were expected and found on all length-scales, depending on the mixing ratio of the two elements. However, not only could the atomic mixing of Fe and Cu be evaluated, but also the distribution of impurities, mostly stemming from the fabrication procedure. The combination of APT and TEM enables a correlation between the structural evolution and the chemical mixing during the milling process.For the first time, a clear distinction can be drawn between the morphological evolution at the surface and in the interior of the powder particles. This became possible owing to the site specific sample preparation of TEM lamellae by Focussed Ion Beam (FIB). Surprisingly, the texture arising from the ball milling process can directly be related to the classical rolling texture of cold rolled Fe.In addition, full homogeneity can be achieved even on the nano-scale for this material as shown by APT, resulting in an extended miscibility region in comparison to the equilibrium phase diagram.Grain sizes were determined by means of XRD and TEM. The strain corrected XRD results are in very good agreement with the values derived by TEM, both confirming a truly nanocrystalline structure.     

Quantitative comparison of energy-filtering transmission electron microscopy and atom probe tomography

Whereas transmission electron microscopy (TEM) is a well established method for the analysis of thin film structures down to the sub-nanometer scale, atom probe tomography (APT) is less known in the microscopy community. In the present work, local chemical analysis of sputtered Fe/Cr multilayer structures was performed with energy-filtering transmission electron microscopy (EFTEM) and APT. The single-layer thickness was varied from 1 to 6 nm in order to quantify spatial resolution and chemical sensitivity. While both the methods are able to resolve the layer structure, even at 2 nm thickness, it is demonstrated that the spatial resolution of the APT is about a factor of two, higher in comparison with the unprocessed EFTEM data. By calculating the influence of the instrumental parameters on EFTEM images of model structures, remaining interface roughness is indicated to be the most important factor that limits the practical resolution of analytical TEM.     

Quantitative atom probe analysis of nanostructure containing clusters and precipitates with multiple length scales

A model Al-3Cu-(0.05 Sn) (wt%) alloy containing a bimodal distribution of relatively shear-resistant θ′ precipitates and shearable GP zones is considered in this study. It has recently been shown that the addition of the GP zones to such microstructures can lead to significant increases in strength without a decrease in the uniform elongation. In this study, atom probe tomography (APT) has been used to quantitatively characterise the evolution of the GP zones and the solute distribution in the bimodal microstructure as a function of applied plastic strain. Recent nuclear magnetic resonance (NMR) analysis has clearly shown strain-induced dissolution of the GP zones, which is supported by the current APT data with additional spatial information. There is significant repartitioning of Cu from the GP zones into the solid solution during deformation. A new approach for cluster finding in APT data has been used to quantitatively characterise the evolution of the sizes and shapes of the Cu containing features in the solid solution solute as a function of applied strain.     

Field-dependent abundances of hydride molecular ions in atom probe tomography of III-N semiconductors

We investigate the microscopic behaviour of hydrogen-containing species formed on the surface of III-N semiconductor samples by the residual hydrogen in the analysis chamber in laser-assisted atom probe tomography (APT). We analysed AlGaN/GaN heterostructures containing alternate layers with a thickness of about 20 nm. The formation of H-containing species occurs at field strengths between 22 and 26 V/nm and is independent of the analysed samples. The 3D APT reconstruction makes it possible to map the evolution of the surface behaviour of these species issued by chemical reactions. The results highlight the strong dependence of the relative abundances of hydrides on the surface field during evaporation. The relative abundances of the hydrides decrease when the surface field increases due to the evolution of the tip shape or the different evaporation behaviour of the different layers.     

Investigation of the analysis parameters and background subtraction for high-k materials with atom probe tomography

In this paper we present depth profiles of a high-k layer consisting of HfO₂ with an embedded sub-nm thick ZrO₂ layer obtained with atom probe tomography (APT). In order to determine suitable measurement parameters for reliable, reproducible, and quantitative analysis, we have investigated the influence of the laser energy and the specimen temperature on the resulting elemental composition. In addition we devise a procedure for local background subtraction both for the composition and the depth scale that is crucial for gaining reproducible results. We find that the composition of the high-k material remains unaffected even for extreme laser energies and base temperatures, while higher laser energies lead to an accumulation of silicon at the upper interface of the high-k layer. Furthermore we show that APT is capable of providing sub-nm depth resolution for high-k materials with high reproducibility, good compositional accuracy, and high measurement yield.     

Atom probe tomography and transmission electron microscopy characterisation of precipitation in an Al-Cu-Li-Mg-Ag alloy

State-of-the art atom probe tomography (APT) combined with transmission electron microscopy (TEM) were used to investigate the microstructure at different stages of the ageing process of an alloy of composition (at%) Al-1.68%Cu-4.62%Li-0.33%Mg-0.1%Ag. These alloys were shown to exhibit a complex microstructure of T₁ plates and several metastable phases, including θ′ and S. We will highlight the early stages of clustering, precipitate interactions and possible solute segregation at the matrix/precipitate interfaces and detail the chemical composition of the different phases.     

Determination of matrix composition based on solute‐solute nearest‐neighbor distances in atom probe tomography

In this study, we propose a fast automatic method providing the matrix concentration in an atom probe tomography (APT) data set containing two phases or more. The principle of this method relies on the calculation of the relative amount of isolated solute atoms (i.e., not surrounded by a similar solute atom) as a function of a distance d in the APT reconstruction. Simulated data sets have been generated to test the robustness of this new tool and demonstrate that rapid and reproducible results can be obtained without the need of any user input parameter. The method has then been successfully applied to a ternary Al‐Zn‐Mg alloy containing a fine dispersion of hardening precipitates. The relevance of this method for direct estimation of matrix concentration is discussed and compared with the existing methodologies. Microsc. Res. Tech., 2010. © 2010 Wiley‐Liss, Inc.     

Multivariate statistical analysis of atom probe tomography data

The application of spectrum imaging multivariate statistical analysis methods, specifically principal component analysis (PCA), to atom probe tomography (APT) data has been investigated. The mathematical method of analysis is described and the results for two example datasets are analyzed and presented. The first dataset is from the analysis of a PM 2000 Fe–Cr–Al–Ti steel containing two different ultrafine precipitate populations. PCA properly describes the matrix and precipitate phases in a simple and intuitive manner. A second APT example is from the analysis of an irradiated reactor pressure vessel steel. Fine, nm-scale Cu-enriched precipitates having a core-shell structure were identified and qualitatively described by PCA. Advantages, disadvantages, and future prospects for implementing these data analysis methodologies for APT datasets, particularly with regard to quantitative analysis, are also discussed.     

Effects of 10 MeV electron irradiation at high temperature of a Ni-Mo-based Hastelloy

A Hastelloy alloy was irradiated with 10 MeV electrons at 650 degrees C for 700 h to a total dose of 2 x 10(-3) displacements per atom (dpa). The microstructure of irradiated and non-irradiated specimens of this alloy were investigated by transmission electron microscopy (TEM). The non-irradiated specimens were analyzed by 3-D atom probe tomography (APT) in a local-electrode atom-probe (LEAP). TEM analysis before the irradiation detects small precipitates with a mean diameter of 22 nm, which are coherent with the FCC matrix. The number density of these precipitates is approximately 7 x 10(18) m(-3). Electron diffraction patterns from these precipitates exhibit superlattice reflections corresponding to the L1(2) ordered structure. The chemical composition of the precipitates, as measured by APT, is around 75 at% Ni with additions of Al, Ti and Mo. After electron irradiation, small precipitates with an irregular morphology are observed. The number density of these new precipitates about 10(20) m(-3) is greater than that of the L1(2) ordered precipitates before irradiation. The L1(2) superlattice reflections disappear completely, instead diffuse diffraction spots are observed at 1(1/2)0(FCC), which is attributed to compositional short-range order (SRO). The results are discussed with respect to the influence of the electron irradiation on the morphology and structure of the ordered precipitates.     

A reproducible method for damage-free site-specific preparation of atom probe tips from interfaces

Atom probe tomography (APT) is a mass spectrometry method with atomic-scale spatial resolution that can be used for the investigation of a wide range of materials. The main limiting factor with respect to the type of problems that can be addressed is the small volume investigated and the randomness of common sample preparation methods. With existing site-specific specimen preparation methods it is still challenging to rapidly and reproducibly produce large numbers of successful samples from specifically selected grain boundaries or interfaces for systematic studies. A new method utilizing both focused ion beam (FIB) and transmission electron microscopy (TEM) is presented that can be used to reproducibly produce damage-free atom probe samples with features of interest at any desired orientation with an accuracy of better than 50 nm from samples that require very little prior preparation.     

Overcoming challenges in the study of nitrided microalloyed steels using atom probe

Nitrided steels are widely used in the engineering field due to their superior hardness and other attractive properties. Atom probe tomography (APT) was employed to study two Nb-microalloyed CASTRIP steels with different N contents. A major challenge of using APT to study this group of materials is the presence of tails after Fe peaks in the mass spectra, which overestimates the composition for alloying elements such as Nb and Cu in the steels. One important factor that contributes to the tails is believed to be delayed field evaporation from Fe²⁺. This artefact of the mass spectrum was observed to be the most severe when voltage pulsing was used. The application of laser pulses with energy ranging from 0.2 to 1.2 nJ successfully reduced the tails and lead to better compositional measurement accuracy. Spatial resolution in the z-direction (along the tip direction) was observed to be less affected by changing laser energy but deteriorates in x-y direction with increasing laser energy. This investigation suggests that pulsed-laser atom probe with ∼0.4 nJ laser energy can be used to study this group of materials with improved mass resolution while still maintaining high spatial resolution.     

Detecting density variations and nanovoids

A combination of simulated and experimental data has been used to investigate the size range of nanovoids that can be detected in atom probe tomography data. Simulated atom probe tomography data have revealed that nanovoids as small as 1 nm in diameter can be detected in atom probe tomography data with the use of iso-density surfaces. Iso-density surfaces may be used to quantify the size, morphology and number density of nanovoids and other variations in density in atom probe tomography data. Experimental data from an aluminum-yttrium-iron metallic glass ribbon have revealed the effectiveness of this approach. Combining iso-density surfaces with atom maps also permits the segregation of solute to the nanovoids to be investigated. Field ion microscopy and thin section atom maps have also been used to detect pores and larger voids.     

Investigation of wüstite (Fe1-xO) by femtosecond laser assisted atom probe tomography

In this paper, we report results obtained from laser assisted three-dimensional (3-D) atom probe tomography (APT) on wüstite (Fe_1−xO). Oxides are generally insulating and hence hard to analyse in conventional electrical assisted APT. To overcome this problem, femtosecond laser pulses are used instead of voltage pulses. Here we discuss some aspects of pulsed laser field evaporation and optimization of parameters to achieve better chemical accuracy.     

Pulsed-laser atom probe studies of a precipitation hardened maraging TRIP steel

A precipitation hardened maraging TRIP steel was analyzed using a pulsed laser atom probe. The laser pulse energy was varied from 0.3 to 1.9 nJ to study its effect on the measured chemical compositions and spatial resolution. Compositional analyses using proximity histograms did not show any significant variations in the average matrix and precipitate compositions. The only remarkable change in the atom probe data was a decrease in the ++/+ charge state ratios of the elements. The values of the evaporation field used for the reconstructions exhibit a linear dependence on the laser pulse energy. The adjustment of the evaporation fields used in the reconstructions for different laser pulse energies was based on the correlation of the obtained cluster shapes to the TEM observations. No influence of laser pulse energy on chemical composition of the precipitates and on the chemical sharpness of their interfaces was detected.     

3-D analysis of semiconductor dopant distributions in a patterned structure using LEAP

This work presents the first 3-D analysis of lateral dopant diffusion in a patterned structure using a pulsed laser-assisted local electrode atom probe (LEAP). A structure similar to a device channel was created for this work by performing a 3 keV, 1×10¹⁵ cm⁻² As⁺ implant on a poly-Si line patterned wafer with 70 nm line width and 200 nm line pitch. The wafer was subsequently annealed at 950 °C for 1 s. LEAP samples were made using a site-selective in-situ focused ion beam (FIB) process. The results from LEAP analysis were then compared with high-resolution transmission electron microscopy (HRTEM) and Florida object-oriented process simulator (FLOOPS) results. Good structural agreement was found between the LEAP and HRTEM results. Several 1-D As concentration profiles extracted from the LEAP data were also found to be in good agreement with FLOOPS process simulation results. These profiles also represent for the first time that results from a 3-D process simulator have been able to be confirmed experimentally using a single sample.     

Gallium-enhanced phase contrast in atom probe tomography of nanocrystalline and amorphous Al-Mn alloys

Over a narrow range of composition, electrodeposited Al-Mn alloys transition from a nanocrystalline structure to an amorphous one, passing through an intermediate dual-phase nanocrystal/amorphous structure. Although the structural change is significant, the chemical difference between the phases is subtle. In this study, the solute distribution in these alloys is revealed by developing a method to enhance phase contrast in atom probe tomography (APT). Standard APT data analysis techniques show that Mn distributes uniformly in single phase (nanocrystalline or amorphous) specimens, and despite some slight deviations from randomness, standard methods reveal no convincing evidence of Mn segregation in dual-phase samples either. However, implanted Ga ions deposited during sample preparation by focused ion-beam milling are found to act as chemical markers that preferentially occupy the amorphous phase. This additional information permits more robust identification of the phases and measurement of their compositions. As a result, a weak partitioning tendency of Mn into the amorphous phase (about 2 at%) is discerned in these alloys.