Quantitative two-dimensional dopant profiles obtained directly from secondary electron images

An international round‐robin test (RRT) was performed to investigate a method to determine the interface location and the layer thickness of multilayer films by secondary ion mass spectrometry (SIMS) depth profiling as a preliminary study to develop a new work item proposal in ISO/TC‐201. Two types of reference materials were used in this RRT. A SiGe alloy (Si 52.4 Ge 47.6 ) reference film was used to determine the relative sensitivity factors of Si and Ge. A Si/Ge multilayer reference film was used to determine the relative sputtering rates of the Si and Ge layers. The layer thicknesses were measured from the interfaces determined by a 50 atomic percent definition. Seven laboratories from 5 countries participated in this international RRT. The RRT reference expanded uncertainties for Si and Ge layers in a Si/Ge multilayer with similar thicknesses as the reference film were 0.76 and 1.17 nm, respectively. However, those in a thinner Si/Ge multilayer film were slightly larger at 1.04 and 1.59 nm, respectively. Most of the thickness ratios in the 2 Si/Ge multilayer films were consistent with the RRT reference value within their expanded uncertainties.

Secondary ion mass spectrometry depth profile analyses were performed on two sets of 4H-SiC(0001) substrate samples implanted with phosphorus. Both sets were processed under the same conditions. We implanted the samples with 100 keV (10(11)-10(14) cm(-2)) phosphorus ions through the thin chemical vapor deposition deposited silicon dioxide stopping mask in order to obtain an ultra-shallow implantation profile. After phosphorus implantation, secondary ion mass spectrometry depth profile analysis was performed on the first set of samples and the second set was subjected to thermal oxidation procedure at 1200 degrees C in order to create a dielectric layer. The aim of the oxidation process was formation of the silicon dioxide layer enriched with phosphorus: the element, which is considered to be suitable for trap density reduction. Ion implantation parameters as well as oxidation and chemical etching procedures were examined for the proper incorporation of phosphorus into the subsurface structure of the silicon oxide. Secondary ion mass spectrometry depth profile analysis was performed with Physical Electronics 06-350E sputter ion gun and QMA-410 Balzers quadrupole mass analyser. The analytical parameters such as: 1.7 keV Ar+ ion beam digitally scanned over 3 x 3 mm(2) area and ion erosion rate of 1.4 nm/min and sampling rate of 0.3 nm, were suitable for samples oxidized after ion implantation.

Two-dimensional dopant profiling is vital for the modelling, design, diagnosis and performance improvement of semiconductor devices and related research and development. Scanning electron microscopy (SEM) has shown great potential for dopant profiling. In this study, the effects of secondary electron (SE) detectors and imaging parameters on the contrast imaging of multilayered p-n and p-i junction GaN specimens via SEM were studied to enable dopant profiling. The doping contrast of the image captured by the in-lens detector was superior to that of the image captured by the side-attached Everhart-Thornley detector at lower acceleration voltages (Vacc ) and small working distances (WD). Furthermore, the doping contrast levels of the in-lens detector-obtained image under different combinations of Vacc and WD were studied, and the underlying mechanism was explored according to local external fields and the refraction effect. The difference in the angular distributions of SEs emitted from different regions, the response of the three types of SEs to detectors, and the solid angles of detectors toward the specimen surface considerably influenced the results. This systematic study will enable the full exploitation of SEM for accurate dopant profiling, improve the analysis of the doping contrast mechanism, and further improve doping contrast for semiconductors.

Ferroelectric SrBi2Ta2O9 (SBT) thin films were prepared on platinized wafer— Pt/TiOx/SiO2/Si— by pulsed laser ablation deposition. Phase formation of SBT film was achieved during the deposition process itself, so the post-annealing that is often used by other groups is not necessary. The SBT film was well-crystallized, showing a dominant (115) peak at a deposition temperature as low as 580 °C, and exhibited good ferroelectric properties— the remanent polarization and coercive electrical field are 7.1 µC cm−2 (2Pr) and 30 kV cm−1, respectively, at an applied electrical field of 80 kV cm−1. Secondary ion mass spectrometry depth profiling and cross-sectional transmission electron microscopy were performed to study the inter-diffusion at the SBT/Pt bottom electrode interface. A sharp SBT/Pt interface was observed at a deposition temperature of 580 °C, but a higher deposition temperature (680 °C) resulted in significant inter-diffusion at the SBT/Pt interface. The formation of a secondary pyrochlore phase was observed due to Ti diffusion into SBT film at a high deposition temperature of 680 °C. Copyright © 1999 John Wiley & Sons, Ltd.

High resolution secondary electron (SE) images can be obtained in a scanning transmission electron microscope (STEM) by collecting the type I secondary electrons generated directly by the incident electron beam. The high resolution SE signal is, in general, localized to about 1 nm in the generation process. The escape depth of the secondary electrons, however, varies from about 1 nm for most metals to about 10 nm for some insulating materials. Surface steps can be imaged by collecting high resolution secondary electrons Among other possible contrast mechanisms for SE imaging of surface steps, topographic contrast plays an important role. The topographic contrast of surface steps depends on: (1) the incident electron probe size; (2) step height to SE escape depth ratio; (3) localization of the generated SE signals and (4) the incident beam angle relative to the specimen surface.In our UHV STEM (MIDAS) instrument, both the entrance and exit surfaces of the sample can be imaged by collecting secondary electrons. For thin samples, the resolution is < lnm for SE images of entrance and exit surfaces but for thicker samples the resolution of the SE image obtained from the exit surface will be degraded by the beam broadening effects. For studying steps on thick or bulk crystal surfaces, secondary electrons emitted from the entrance surfaces are, in general, collected to form images with high contrast and high resolution. In this report, all the SE images are obtained, in MIDAS, by collecting secondary electrons emitted from the entrance surfaces of the samples. Figure 1 is a SE image of a MgO smoke crystal revealing the surface growth steps with high contrast. The parallel straight steps, along <100> directions, constitute the edges of unfinished atomic planes on the MgO {100} crystal surfaces. This image indicates that the {100} surfaces of MgO smoke crystals are flat surfaces. Figure 2 shows a SE image of a MoO3 crystal with surface growth steps spiraling from an end-on screw dislocation (the black dots in the SE image represent electron beam induced reduction products). The dark lines (indicated by D) represent up-steps and the bright lines (indicated by B) represent down-steps. It is interesting to note that the two-dimensional crystal growth around the dislocation is anisotropic, forming terraces with long edges parallel to [010] direction.

In this paper the origin of the carbide/matrix contrast in secondary electron images and its ramifications for spatial resolution are investigated. A profound influence of the backscattered electron yield and the oxidation of the steel matrix was found, which manifests itself in a contrast reversal at low primary electron beam energies. The authors established that low beam energies are necessary to obtain the required spatial resolution. Strategies for optimizing the contrast between carbide and matrix in secondary electron images without compromising the spatial resolution are presented. A simple method to estimate the thickness of thin oxide layers from low voltage secondary electron images is also described.

The complementary metal-oxide-semiconductor (CMOS) industry continues to push the boundaries of what is possible. Along with this, secondary ion mass spectrometry (SIMS) depth profiling continues to support CMOS R&D and high volume manufacturing (due to its unparalleled sensitivity and detection limits over predefined volumes and within acceptable time periods). New developments in SIMS are also being realized to support the move of the CMOS industry from planar structures to three-dimensional (3D) structures. This article presents a perspective of existing SIMS research areas for beyond one-dimensional structural analysis along with potential future SIMS implementation and data processing scenarios. The topics covered include: (1) existing SIMS depth profiling approaches for 3D structures, (2) in-fab SIMS deployment, (3) data analysis of in-fab SIMS derived depth profiles from 3D structures via pattern recognition, and (4) hybrid characterization approaches. With SIMS depth profiling of optimized (for SIMS) 3D structures already demonstrated, the remaining topics may serve to extend these and other capabilities and open new application areas for SIMS.

We have grown stoichiometrically thin films of the narrow bandgap semiconductor Bi2Te3 by molecular beam epitaxy in an ultra-high vacuum on single-crystal substrate Sb2Te3 in order to optimize the growth conditions for this technique. High resolution X-ray diffraction, scanning electron microscope observations and energy dispersive X-ray spectroscopy analysis are used to characterize the substrate and the deposited layers. In addition, secondary ion mass spectroscopy depth profiling is used to study the diffusion and the concentration profiles of layer elements. We have also studied the effect of heat treatment on some of the electrical properties of single-crystal substrate as a function of temperature in order to analyse its semiconducting behaviour at low temperature. The sticking coefficients Ks(Te) and Ks(Bi) of the elements Te and Bi, respectively, are determined as a function of substrate temperature Ts and flux ratio FR = [F(Te)/F(Bi)]. It is found that Ks(Te) is very sensitive to both Ts...

For a better comprehension of hydrogen intercalation of graphene grown on a silicon carbide substrate, an advanced analytical technique is required. We report that with a carefully established measurement procedure it is possible to obtain a reliable and reproducible depth profile of bi-layer graphene (theoretical thickness of 0.69 nm) grown on the silicon carbide substrate by the Chemical Vapor Deposition method. Furthermore, we show that with depth resolution as good as 0.2 nm/decade, both hydrogen coming from the intercalation process and organic contamination can be precisely localized. As expected, hydrogen was found at the interface between graphene and the SiC substrate, while organic contamination was accumulated on the surface of graphene and did not penetrate into it. Such a precise measurement may prove to be invaluable for further characterization of 2D materials.

We have used cross-sectional micro-Auger electron spectroscopy (AES), coupled with micro-cathodoluminescence (CLS) spectroscopy, in a UHV scanning electron microscope to probe the chemical and related electronic features of hydride vapor phase epitaxy GaN/sapphire interfaces on a nanometer scale. AES images reveal dramatic evidence for micron-scale diffusion of O from Al2O3 into GaN. Conversely, plateau concentrations of N can extend microns into the sapphire, corresponding spatially to a 3.8eV defect emission and Auger chemical shifts attributed to Al-N-O complexes. Interface Al Auger signals extending into GaN indicates AlGaN alloy formation, consistent with a blue-shifted CLS local interface emission. The widths of such interface transition regions range from <100nmto∼1μm, depending on surface pretreatment and growth conditions. Secondary ion mass spectroscopy depth profiles confirm the elemental character and spatial extent of diffusion revealed by micro-AES, showing that cross-sectional AES is a useful approach to probe interdiffusion and electronic properties at buried interfaces.

The use of aluminum as an electrode in metal-insulator-semiconductor devices containing lanthanum oxide is impaired by unacceptable leakage current levels. Time of flight secondary ion mass spectroscopy depth profiling shows a significant amount of silicon out-diffusion from the substrate and aluminum in-diffusion towards the oxide. By using titanium nitride as the electrode, the silicon out-diffusion is suppressed, which improves the device performance. This indicates that, despite the larger coordination number of the lanthanum ions in the oxide, aluminum acts as a sink for silicon, thus driving the out-diffusion of silicon.

A laser-assisted plasma etch process is presented as an alternative to reactive ion etching for Si wafer processing in upcoming integrated circuit technology nodes. Poly-Si films were etched using an upstream 13.56 MHz inductively coupled plasma source while simultaneously being exposed to a pulsed Nd:YAG laser using the 532 nm line, with 100 Hz and 7 ns Gaussian pulse duration. For a fluorocarbon etch recipe of 50:8 sccm Ar:C4F8 with varied O2 flow, a minimum laser intensity for etch onset was necessary to overcome CFx polymer deposition in the absence of substrate bias. This etch onset occurred at 20 ± 3 mJ/cm2/pulse for 0 sccm O2 flow, dropping to 8 ± 2 mJ/cm2/pulse for 1.5 sccm O2. Beyond this onset, the etch rate increased linearly with laser intensity. Secondary ion mass spectroscopy depth profiling data showed that the no-bias 532 nm laser-assisted etch process preserved the distinction between the Si surface and the CFx polymer, with minimal uptake of etch gas residuals (C/F/O) in the Si. On the other hand, RIE showed significant straggle of the Si layer, spreading 3.5 nm through the CFx polymer layer at 1.0 W/cm2 radio-frequency bias and −140 V direct self-bias. comsol modeling of 532 nm incident on 22 nm half-pitch trench features showed strong polarization dependence, with deep-trench heating possible with polarization perpendicular to the trench line. This effect was confirmed in brief laser-assisted SF6 etching of pre-existing 50 nm half-pitch linear trenches.

We report the implementation of recent advances in metalorganic chemical vapor deposition (MOCVD) for in situ growth of four-layer HgCdTe mid wave/ long wave (MW/LW) simultaneous dual-band 64 × 64 infrared detector arrays. This independently accessed, simultaneous, double-heterojunction p-n-N-P dualband detector has two back-to-back stacked photodiodes grown on CdZnTe (100) substrates. The LW photodiode is a p-on-n heterojunction grown on top of an MW N-on-P heterojunction photodiode. Secondary ion mass spectrometry depth profiles of these 28 µ m thick p-n-N-P dual-band films show four well-defined regions of alloy composition and doping, and agree well with the device design. 64 × 64 arrays of dual-band detectors were fabricated from these films using electron cyclotron resonance dry etching and CdTe passivation, and hybridized to a dual-band readout chip. Two bump inter-connects in each unit cell provide independent electrical access to the back-to-back MW and LW photodiodes, and allow the MW and LW photocurrents to be separate and independent. The dualband infrared focal plane arrays (IRFPAs) spectral response data at 78K are well-behaved and are fully consistent with that observed in individual singleband LW p-on-n and MW N-on-P heterojunction devices of the same design. The hybridized 64 × 64 duai-band FPAs have MW and LW average in-band quantum efficiencies of 79 and 67%, and median D* values of 4.8 × 1011 and 7.1 × 1010 cm-√Hz/W, in the respective spectral bands at 78K. The data demonstrate that MOCVD has progressed significantly toward being a practical and viable vapor phase in situ growth technology for advanced bandgap-engineered HgCdTe detector arrays.

We have investigated the residual stress distribution and its relation to the presence of impurity atoms in InP layers grown by metalorganic vapor phase epitaxy (MOVPE) on top of lattice-matched GaInAs layers. The homogeneous and gradient components of the stress have been directly measured using highly sensitive micromechanical test structures. Secondary ion mass spectrometry depth profiling of the composition evidenced that residual As and Ga atoms are present throughout the relatively thick (>0.5 μm) InP layers. Our investigations show that the distribution of these impurities accounts for the measured residual stress in the layers and, at the same time, it is specific to the MOVPE growth technique.

We report ALD-Ru thin films using a new carbonyl-based Ru precursor and compare the results with various nonoxidizing reactants such as H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> , NH <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">3</sub> , CO molecule and NH <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">3</sub> , N <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> , H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> , N <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> +H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> mixture plasma. In addition, we also investigated ALD-Ru process with post annealing and in-situ periodic plasma treatment to improve ALD-Ru film quality. The Ru film was deposited at the deposition temperature ranging from 100 to 150 °C and at the chamber pressure from 1 to 50 Torr. In the case of using N <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> and H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> mixture plasma as a reactant, it was possible to deposit Ru film even at a substrate temperature of 100°C and the film resistivity of ~ 70 μΩ·cm was deposited after annealing and in-situ plasma treatment. It was shown that ALD-Ru film with the resistivity of ~ 25 μΩ·cm could be prepared using H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> molecules at 150°C with increasing chamber pressure up to 30 Torr. The step coverage of ALD-Ru films deposited using H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> molecules and at the chamber pressure of 30 Torr was excellent, around 100 % at dual trench structure with aspect ratio of ~ 6.3. It should be noted that ALD-Ru films deposited using H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> molecules contained no oxygen and carbon impurities while Ru films using deposited diluted O <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> has oxygen and carbon impurities by secondary ion mass spectrometry depth profile. And electro-plating of Cu is successfully possible on ALD-Ru deposited using H <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> molecules at 30 Torr.