Experimental observation of FIB induced lateral damage on silicon samples

In this paper, we present our recent applications of scanning capacitance microscopy (SCM) on specific devices with sampling window as small as 100nm. The dopant related root causes were successfully identified on those devices fabricated with 90nm CMOS technology. The key step in our approach is the development of a sample preparation technique that allows us to precisely x-section through a transistor without being affected by focused ion beam (FIB) artifacts. FIB was used to mark the area of interest with high precision, but it did not expose the devices of interest. Optical microscope and atomic force microscope (AFM) were used to inspect the mechanically polished surface, thus avoiding beam effects from FIB or SEM. In the first application, a doping anomaly was identified in a PFET poly gate, in a single bit failed SRAM cell. In the second application, an asymmetry of a PWell implant profile in a window of 150nm was identified as the cause of leakage in a capacitor array. Our approach may be applied to other scanning probe microscopy (SPM) techniques in the same category, i.e., scanning spreading resistance microscopy (SSRM) or scanning microwave microscopy (SMM).

The availability of very sharp, wear-proof, electrically conductive probes is one crucial issue for conductive atomic force microscopy (AFM) techniques such as scanning capacitance microscopy, scanning spreading resistance microscopy, and nanopotentiometry. The purpose of this systematic study is to give an overview of the existing probes and to evaluate their performance for the electrical techniques with emphasis on applications on Si at high contact forces. The suitability of the characterized probes has been demonstrated by applying conductive AFM techniques to test structures and state-of-the-art semiconductor devices. Two classes of probes were examined geometrically and electrically: Si sensors with a conductive coating and integrated pyramidal tips made of metal or diamond. Structural information about the conductive materials was obtained by electron microscopy and other analytical tools. Swift and nondestructive procedures to characterize the geometrical and electrical properties of the probes prior to the actual AFM experiment have been developed. Existing contact models have been used to explain variations in the electrical performance of the conductive probes.

We used scanning capacitance microscopy (SCM) and scanning spreading resistance microscopy (SSRM) to determine the drift hole mobility in nanometer thick Si∕Si0.75Ge0.25∕Si quantum wells (QWs), from the carrier concentration profiles (obtained by SCM) and the local resistivity values (obtained by SSRM). A relevant decrease of the hole mobility at room temperature was observed when reducing the QW width from 10 nm down to 1 nm. This effect has been explained in terms of the increasing role of surface scattering at the Si∕SiGe interface for lower QW widths.

Evaluation of scanning capacitance microscopy sample preparation by focused ion beam

Different techniques based on the atomic force microscope (AFM) have been developed in the last few years for the electrical characterization of semiconductor devices. The quality of these measurements strongly depends on the tip which should not only have a small radius of curvature but also a high electrical conductivity. Therefore, the choice of metal as tip material is obvious. We have developed a process scheme for the fabrication of pyramidal metal tips which are integrated into a silicon cantilever. This paper discusses this process in detail and shows how the transition was made from prototyping to batch friction using standard 150 mm silicon wafer technology. Results are presented concerning the application of such probes for two-dimensional carrier profiling of InP and silicon structures using scanning spreading resistance microscopy (SSRM) and scanning capacitance microscopy (SCM). A novel tip configuration called tip-on-tip has also been developed. This concept looks promising for future applications. We demonstrate how such a tip-on-tip configuration can be realized.

Scanning spreading resistance microscopy (SSRM) has been applied to study focused ion beam (FIB) induced damage in silicon in dependence on ion irradiation doses from 1012 cm-2 to 2·1016 cm-2. Starting from the lowest dose, SSRM detects increasing spreading resistance (SR) with increasing dose. For doses from 2·1013 cm-2 to 4·1014 cm-2, a slight decrease of SR is measured whereas for higher doses SR again slightly increases. The results are explained by physical effects like decreased carrier mobility due to increased scattering, amorphisation of silicon and precipitation of implanted Ga ions. The results clearly prove that SSRM is well suited for the fast detection of ion beam induced damage with high lateral resolution.

Scanning capacitance microscopy (SCM) is based on a contact-mode variant of atomic force microscopy, which is used for imaging two-dimensional carrier (electrons and holes) distributions in semiconductor devices. We introduced a method of quantification of the carrier concentration by experimentally deduced calibration curves, which were prepared for semiconductor materials such as silicon and silicon carbide. The analytical procedure was circulated to research organizations in a round-robin test. The effectiveness of the method was confirmed for practical analysis and for what is expected for industrial pre-standardization from the viewpoint of comparability among users. It was also applied to other electric scanning probe microscopy techniques such as scanning spreading resistance microscopy and scanning nonlinear dielectric microscopy. Their depth profiles of carrier concentration were found to be in good agreement with those characterized by SCM. These results suggest that our proposed method will be compatible with future next-generation microscopy.

Heavily n-doped epitaxially grown Si layers are of great importance for source/drain (S/D) application in advanced node nMOS devices. For contact resistivity reduction, the dopant activation level is very important. Various techniques are being used to evaluate dopant activation in Si:P layers. Among these two methods are Scanning Spreading Resistance Microscopy (SSRM) and Differential Hall Effect Metrology (DHEM). SSRM uses an atomic force microscope equipped with a hard conductive probe that is scanned in contact mode on the cross-sectioned sample’s surface and measures spreading resistance. Measured resistance values as a function of depth are converted into resistivity and carrier concentration depth profiles using calibration measurements and conversion relationships. DHEM provides depth profiles of mobility, resistivity and carrier concentration through a semiconductor layer by making successive sheet resistance (Rs) and Hall voltage measurements using Hall effect/Van der Pauw techniques, as the electrically active thickness of the layer is reduced through successive oxidation steps. Controlled oxidation is achieved by electrochemical anodization. Data collected can then be processed to yield the depth profiles. In this contribution we have carried out SSRM and DHEM measurements on Si:P epi layers subjected to different processing conditions including annealing and ohmic contact fabrication. Secondary Ion Mass Spectrometry (SIMS) was used to measure the total (active + inactive) dopant profiles through the films. Effects of these processes on dopant diffusion and activation were studied and the results from DHEM and SSRM were compared.In-situ phosphorus (P) doped Si epi-layers were grown over 300mm diameter boron doped monitor wafers. While one set was kept as the reference, a second set was treated by a spike-annealing process at 1000 °C. In a third set a Ti/TiN contact fabrication process was carried out and the contact was removed before analysis. In the fourth set contact process was applied to the spike annealed wafer before removal of the Ti/TiN layers. Bulk sheet resistance measurements were made using 4-point probe (4PP) for all the samples. SSRM measurements were carried out at IMEC. Cross-shaped Van der Pauw test-patterns were formed on 8mmx8mm areas on the samples and DHEM measurements were performed at ALP. Figure below shows the dopant depth profiles obtained by SIMS and the carrier concentration profiles from DHEM and SSRM techniques for samples D02 (as deposited Si:P) and D03 (spike annealed). One can make some general observations from the data in this figure. The total dopant concentration as measured by SIMS is ~ 1.4E21/cm3. There is only a small difference in the total dopant distribution profiles (SIMS) between the as deposited sample and the spike annealed sample. However, the spike annealed sample shows much higher dopant activation as measured by DHEM. Carrier concentration is ~2.5x higher in sample D03 (~5E20/cm3) compared to sample D02 (~2E20/cm3). Activation levels measured by SSRM, however, are lower for both samples, and the peak carrier concentration value increases only slightly upon spike annealing, going from ~2E20/cm3 in sample D02 to ~2.2E20/cm3 in sample D03. DHEM clearly indicates the sharp interface between the p-type substrate and the n-type epi-layer and its depth calibration agrees well with the expected thicknesses of the epi layers. The tail of the SSRM data is much more graded. Data from other samples will be presented and discussed in the final manuscript. Figure 1

This paper reviews some recent advances in the application of scanning probe microscopy (SPM) electrical characterization techniques to several critical surface and interface issues in SiC technology. High resolution carrier profiling capabilities in SiC of scanning capacitance microscopy (SCM) and scanning spreading resistance microscopy (SSRM) were employed for several applications. These included two-dimensional (2D) imaging of doped regions in SiC devices (to be used as input for device simulations or as a feedback for device processing) and the quantitative evaluation of the electrically active profiles of P (or N) and Al implanted 4H-SiC after high temperature treatments. Furthermore, the electrical modification of the SiO2/4H-SiC interface in MOS devices subjected to post-oxide-deposition treatments in NO or N2O and POCl3 have been investigated, providing quantitative information on the electrical activation of incorporated N or P in the few-nm-thick SiC interfacial region. The lateral homogeneity of metal/SiC interfaces was probed at nanoscale by conductive atomic force microscopy (CAFM), with a special emphasis given to the case of Schottky contacts on 3C-SiC, where the diode behaviour is strongly affected by the high density of electrically active defects in the substrate. Finally, CAFM has been employed to study the current transport in epitaxial graphene (EG) grown on 4H-SiC (0001), revealing the impact of the substrate morphology (terraces and steps or facets) on the local conductivity.

This paper explores the use of secondary electron (SE) doping contrast in scanning electron microscopy (SEM) for visualizing and quantifying doping in silicon carbide (SiC), a vital wide bandgap semiconductor for power electronics. Traditional methods, such as scanning spreading resistance microscopy and scanning capacitance microscopy, face challenges with SiC due to its high hardness. We propose a theoretical model based on potential differences between n- and p-doped areas, differing from the conventional surface band bending theory. The experimental data align well with our model, revealing insights into SE yield variations due to doping concentrations. The study also examines surface patch fields above p–n junctions and the effect of sample bias on SE yield, differentiating the impacts of surface band-bending and external patch fields. Our findings show strong agreement between theory and experiment, explaining contrast characteristics in energy-filtered secondary electron images. This work enhances the understanding of doping contrast mechanisms in SEM, enabling the development of a quantitative dopant profiling method for SiC.

Selective area growth (SAG) of gallium nitride (GaN) on silicon (Si) wafers efficiently relaxes the tensile stress that is generated in the GaN layer, when the structure is cooled down to room temperature after the growth. Hence, SAG enables the growth of thicker layers that are capable of operating at higher voltages than those grown in 2D layers. In this study, two GaN layers are grown by SAG on 200 mm-diameter Si(111) wafers by metal organic vapor phase epitaxy for the fabrication of pseudo-vertical p–n diodes. During the growth, the SiH4 precursor flow for the first sample was double than that for the second one. The uniformity of the doping concentration of the layers is investigated by scanning spreading resistance microscopy and the p- and n-type doped regions are examined by scanning capacitance microscopy. A low net doping concentration of 1.4 × 1016 cm−3 is extracted from capacitance–voltage measurements and a destructive breakdown occurs at 700 V for a 90 μm-diameter pseudo-vertical p–n diode. These results show the high potential of the SAG of GaN on Si wafers for vertical power devices.

The extended InGaAs short wavelength infrared (SWIR) detector covers 1.0-2.5 μm wavelength, which plays an important role in weather forecast, resource observation, low light level systems, and astronomical observation and so on. In order to fabricate the high performance extended InGaAs detector, materials structure and parameters were characterized with Scanning Capacitance Microscopy (SCM), Scanning Spreading Resistance Microscopy (SSRM), the spreading of minority carriers and lattice quality were obtained. Mesa etching process, etching damage restoration technique and low temperature passivation technique were used in the fabrication of the extended InGaAs detector. The improvement of material structure and device process was studied by fabricating and measuring different perimeter-to-area (P/A) photodiodes and singledevice, respectively. The dark current density of the extended InGaAs detector obviously was reduced, about 2 nA/cm2 at 170 K. The 512×256 FPAs were fabricated, the peak detectivity and the quantum efficiency of which are 5×1011 cmHz1/2/W and 80%, respectively. The staring image yielded of the 512×256 FPAs is shown, which demonstrates very good imaging quality.

Magnetic force microscopy has the capability to detect magnetic domains from a close distance, which can provide the magnetic force gradient image of the scanned samples and also simultaneously obtain atomic force microscope (AFM) topography image as well as AFM phase image. In this work, we demonstrate the use of magnetic force microscopy together with AFM topography and phase imaging for the characterization of magnetic iron oxide nanoparticles and their cellular uptake behavior with the MCF7 carcinoma breast epithelial cells. This method can provide useful information such as the magnetic responses of nanoparticles, nanoparticle spatial localization, cell morphology, and cell surface domains at the same time for better understanding magnetic nanoparticle-cell interaction. It would help to design magnetic-related new imaging, diagnostic and therapeutic methods.

Scanning spreading resistance microscopy (SSRM) is a powerful technique for quantitative two-and three-dimensional carrier profiling of semiconductor devices with sub-nm spatial resolution. However, considering the sub-10 nm dimensions of advanced devices and the introduction of three-dimensional architectures like fin field effect transistor (FinFET) and nanowires, the measured spreading resistance is easily impacted by parasitic series resistances present in the system. The limited amount of material, the presence of multiple interfaces, and confined current paths may increase the total resistance measured by SSRM beyond the expected spreading resistance, which can ultimately lead to an inaccurate carrier quantification. Here, we report a simulation assisted experimental study to identify the different parameters affecting the SSRM measurements in confined volumes. Experimentally, the two-dimensional current confinement is obtained by progressively thinning down uniformly doped blanket silicon on insulator wafers using scalpel SSRM. The concomitant SSRM provides detailed electrical information as a function of depth up to oxide interface. We show that the resistance is most affected by the interface traps in case of a heterogeneous sample, followed by the intrinsic resistance of the current carrying paths. Furthermore, we show that accurate carrier quantification is ensured for typical back contact distances of 1 μm if the region of interest is at least nine times larger than the probe radius.

Recently, we reported significantly improved spatial resolution in scanning spreading resistance microscopy (SSRM) by measuring in a vacuum. In this work, we demonstrate the 1-nm-spatial resolution of SSRM on pn junction delineation by comparing with three-dimensional device simulation. A five-order dynamic range of carrier concentration is also confirmed on staircase sample. A systematic comparison between pFETs/nFETs on (110) and (100) substrates has been carried out with SSRM. The S/D of (110) pFETs shows less lateral distribution than that of (100), strongly indicating 2D-channeling effect of boron ion implantation. We also succeeded in a new sample-making method by fully FIB pick up, enabling site-specific SSRM characteristics for failure analysis and for further scaled devices.