International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 Nanoscopic Study of HfO2 Based HK Dielectric Stacks and Its Failure Analysis K. Shubhakar Singapore University of Technology and Design, 20 Dover Drive, Singapore 138682 Division of Microelectronics, School of Electrical and Electronic Engineering, Nanyang Technological University, 50 Nanyang Avenue, Singapore 639798 Email: [email protected] N. Raghavan and K. L. Pey Singapore University of Technology and Design, 20 Dover Drive, Singapore 138682 Email: {Nagarajan.raghavan, peykinleong}@sutd.edu.sg Abstract—In this invited paper, we present local electrical characteristics, degradation phenomenon and breakdown analysis of polycrystalline HfO2 dielectric stacks at nanometer scale resolution. Grain boundaries (GBs) in polycrystalline high-κ (HK) dielectric films play a major role in the performance and reliability metrics of HK based advanced metal-oxide-semiconductor (MOS) devices. Hence, it is important to study the degradation and breakdown phenomenon in polycrystalline HfO2 dielectric stacks. The nanoscale localized dielectric breakdown (BD) events are analysed using conductive-atomic force microscopy (C-AFM) and transmission electron microscopy (TEM) techniques. Results show an enhanced trap generation and faster degradation of polycrystalline HfO2 gate dielectrics at GB sites as compared to the bulk (grain) regions. A new technique is adopted to induce the degradation and BD of the HfO2 dielectric locally using a combined scanning tunnelling microscopy/scanning electron microscopy nanoprobing system. This method of analysis is very useful in studying the nature of the breakdown events in dielectrics, elucidating the structural changes of the dielectric and the role of the gate electrode in dielectric BD events. resolution [6]-[9]. Again, identification of the BD locations is one of the major issues in the study of failure analysis of MOSFETs. Therefore, special techniques to identify and analyse the BD sites at a nanometer resolution are required to investigate the nature of localized degradation and BD of the dielectric in detail. Here we demonstrate the combined study of conductiveAFM (C-AFM) and the transmission electron microscopy (TEM) analysis of the degradation and BD in nanometer resolution. II. In this work, C-AFM has been used to characterize the morphology and local electrical properties of HfO 2/SiOx dielectric stack. AFM experiments were carried out in ultra-high vacuum (~10–10 Torr). The conducting Pt-wire AFM tip (apex diameter ~50nm) acts as a top gate measures the leakage current across the dielectric at every pixel while scanning for the topographical image, with a constant voltage bias applied to the sample. The tip was always grounded while a bias was applied to the sample. Hence, the topographical and electrical properties of the dielectric can be collected simultaneously at a nanometer scale. Current-stress time (I-t) studies were also carried out at different locations on the polycrystalline HfO 2 dielectric. Annealed (600°C) HfO2 (~4nm)/SiOx (~1nm)/Si samples, which were fabricated using atomic layer deposition technique, were used. A technique that combines scanning electron microscopy (STM) and scanning electron microscopy (SEM) with nano-probing facility was also used in our work to induce the localized BD on HfO2/SiOx dielectric stack. Electron-beam patterned Au (~80nm)/Ti (~5nm) gate electrodes were fabricated on HfO2/SiOx dielectric stacks and these devices were subjected to a STM tip induced ramped voltage stressing (RVS) for the BD events under constant height mode STM operation. This was followed by focused ion-beam sample preparation to carry out TEM analysis. Fig. 1 shows the cross-sectional TEM micrographs of metal/HfO2 (~5nm)/SiOx (~1nm)/Si structure. Index Terms—dielectric, grain conductive-AFM, breakdown I. boundary, high-κ, INTRODUCTION The degradation and failure of high-κ (HK) dielectrics would be a major challenge for the reliability of HKbased CMOS technology. In MOS structures, the conventional electrical tests at device level do not provide the complete physical analysis of the localized percolation path formation and subsequent breakdown (BD) events in dielectrics. The formation of the conductive percolation path and eventual dielectric BD events are localized [1]-[7]; it is therefore essential to study these phenomena with nanometer resolution to analyse the overall reliability and failure of advanced HK gate dielectric stacks. Atomic force microscopy (AFM) technique is used extensively as a tool for the characterization of HK dielectrics with nanometer Manuscript received November 11, 2013; revised February 15, 2014. ©2014 Engineering and Technology Publishing doi: 10.12720/ijmse.2.2.81-86 EXPERIMENTS 81 International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 Figure 1. Cross-sectional TEM micrograph of HfO2 (~4nm)/SiO2 (~1nm) on Si-substrate, annealed at 600°C, showing the polycrystalline HfO2 dielectric. III. Figure 3. Weibull plot of TDDB for C-AFM induced BD locations (~20) in the HfO2/SiOx stack [7]. RESULTS AND DISCUSSIONS A. HfO2 Dielectric Degradation and Breakdown Analysis There are a few reports relating to higher leakage current at the GB sites of polycrystalline HfO2 dielectrics [10]-[13]. Grain boundaries (GBs) in polycrystalline HK dielectrics contain a high density of defects which favoring an accumulation of more traps, leading to the formation of a percolation path [10], [11]. We directly address this issue using C-AFM experiments and simulations in this section. Fig. 2(a) and Fig. 2(b) show a C-AFM topographical image and the corresponding current map, showing the grains and their GB contours. A higher leakage current, i.e., bright spots on the current map at the GB locations, was observed corresponding to the depressed locations on the topographical image, indicating the enhanced trapassisted tunneling (TAT) through the high concentration of pre-existing traps present at the GBs [10]-[12]. Fig. 2(c) shows a line profile of the topography and current map along the line X1-X2 depicting an increase in the leakage current at the GB locations. Figure 4. Simulated failure time distribution for (a) amorphous and (b) polycrystalline HK thin film of thickness. Higher localized trap generation rate at the GB causes the distribution to be non-Weibull [14]. A localized leakage current evolution with stress time under constant voltage stressing (CVS) of +6V, at different locations (grain and GB regions), was performed. During the CVS test, the C-AFM tip was maintained over a location for a specific period of time with a constant voltage applied between the tip and the sample. Fig. 3 shows the Weibull probability plot of the time-dependent dielectric breakdown (TDDB) distribution for C-AFM induced localized BD events of HfO2/SiOx dielectric stack at ~20 different locations. The results clearly show a convexial distribution, with steeper low percentile and shallower high percentile trends [7]. This non-linearity is more likely due to the GB defects present in the HK dielectric. The Weibull plots of simulated (Kinetic Monte Carlo) time-to-failure (TTF) distribution for an amorphous and polycrystalline HfO2 film are used to analyse the failure distribution in HK dielectrics. Fig. 4 shows the simulated time to failure (TTF) distribution for an (a) amorphous and (b) polycrystalline HfO2 film (with κGB = 26 (dielectric constant at GB region) > κG = 25 (dielectric constant at grain region)) [14]. The amorphous stack shows a linear trend in the Weibull scale clearly representative of the standard Weibull distribution (Fig. 4(a)). However, the polycrystalline microstructure shows convexial trends (Fig. 4(b)) with steeper low percentile and shallower high percentile trends [14]. Since the only parameter change in these two cases is κGB ≠ κG, it can be implied that non- Figure 2. (a) C-AFM topography, (b) corresponding C-AFM current map (at +5V) of HfO2 gate dielectric depicting the grain and GB profile. (c) Line profile of topography and C-AFM current map along line “X1X2” shown in (a) and (b). ©2014 Engineering and Technology Publishing 82 International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 The nanometer scale C-AFM results correlate well with the GB assisted BD phenomenon evidence in device level HfO2/SiOx dielectric stacks as shown in Fig. 7 [15]. Bright contrast lines along the GB region in the TEM cross-section of the failed NMOS device is clearly observed along with dielectric breakdown induced epitaxy (DBIE) microstructural defects, pointing to the preferential occurrence of failures at the proximity of the GB site [15]. Fig. 8 shows the schematics of higher electric field at IL below the GB, GB degradation effect on IL and its breakdown phenomenon. uniform localized trap generation leads to the convexial TTF distribution trends. The extent of defectivity in the GB therefore plays a major role in governing the shape of the statistical distribution [14]. Weibull plot of TDDB for C-AFM data is in good agreement with the simulation results. The impact of uniform electrical stress was analyzed on polycrystalline HfO2 dielectric using C-AFM. Fig. 5(a) and Fig. 5(b) show the topography and current map in the first scan obtained at +6V, respectively. Fig. 5(c) and Fig. 5(d) show the current maps over the same area in the second and third scans, respectively, obtained at +6V. The magnitude of the leakage current and conducting region along the GB increases upon uniform stressing, indicating a higher rate of stress induced trap generation compared to the grain regions. Fig. 6 shows the line profile of topography and current maps along the line “XY” in Fig. 5. Results clearly indicate higher increase in the leakage current and faster degradation along the GBs upon stressing. Hence, these conductive percolation paths could evolve into BD spots. Underlying the GB, the thin SiOx interfacial layer (IL) region experiences enhanced local electric field due to a lower electrical resistance in the GB path, causing stress-induced traps to be generated within the IL, resulting in the degradation and BD of the IL layer, which could further enhance the degradation rate locally at that particular GB location [7]. Figure 7. TEM cross-section of a GB site failure in the HfO2 HK layer along with DBIE [15] Figure 8. Schematics of the proposed BD sequence in HK/IL dielectric stack. (a) Higher electric field at IL below the GB (rectangular box in yellow), (b) further increased electric field at IL below the degraded GB upon stressing (rectangular box in red), and (c) IL BD in HK/IL dielectric stack (small circles represent the traps in the dielectric) [7]. To induce a localized BD in tip injection mode, a specific location on the HfO2 dielectric was selected and subjected to localized stressing by maintaining the conductive AFM tip at a location with a bias applied between tip and sample. The C-AFM topographic (Fig. 9(a)-(c)) and corresponding current images (Fig. 9(d)-Fig. 9(f)), show the evolution of a localized BD event. Fig. 9(a) and Fig. 9(d) show the C-AFM topography and current image (at +6V) of the HfO2/SiOx dielectric stack, respectively, before stressing. A location on the HfO2 dielectric marked in dotted circle was subjected to a CVS at +7V (tip injection) locally until the BD event occurred. Fig. 9(b) and Fig. 9(e) show the topographic and current images after the BD event, respectively. No topographical change was observed at the stressed location, indicating no structural deformation occurred during the BD event, but the conductivity at the stressed location increased significantly as observed in the current image (Fig. 9(e)). Inducing further stressing at the same location leads to significant structural changes and current at the BD spot. The formation of the depression/void at the BD spot was observed in the surface topography as shown in Fig. 9(c). The field-induced rupture of the HfO2/SiOx dielectric stack in the direction of electron wind could be the possible reason for the formation of depression at the BD spot. Fig. 9(f) shows the corresponding current image of the hard-BD (HBD) spot presenting highly conductive region (dotted circle in Fig. 9(f)) [6]. Figure 5. (a) C-AFM topography and leakage current profile at +6V after the (b) 1stscan, (c) 2ndscan, (d) 3rd scan of a HfO2/SiOx sample [7]. Figure 6. The line profile of topography and corresponding line profile of the current maps during uniform stressing along the line “X-Y” shown in Fig. 5 [7] ©2014 Engineering and Technology Publishing 83 International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 11(b) and Fig. 11(c) show the high-resolution (HR)-TEM and scanning TEM (STEM) micrographs of the BD region marked in Fig. 11(a). The dielectric is still intact, where no punch through was found. The migration of Au/Ti gate electrode material occurs at the BD region due to the dielectric breakdown induced metal migration [18], [19], forming a low resistance path between the gate and Si substrate triggering the failure of the device. A “ballshaped” capping layer was formed at the Si substrate and it was observed that the ball-shaped capping layer induced by BD was found to be composed of gate electrode material as presented in an elemental mapping in Fig. 11(d), obtained at a spot marked by a dot in the capping layer (Fig. 11(c)) [6]. Figure 9. (a)-(c) C-AFM topography profile at different stages of localized degradation and breakdown under tip injection. (a) and (d) are pre-stress results. Images (d)-(f) are the corresponding current maps for (a)-(c) at +6V. The inset of (c) is the line profile of the topography at the BD area [6]. B. STM Tip Induced Localized BD Analysis Most of the analysis of the BD phenomenon of HfO2/SiOx dielectric stack in the literature is based on device-level electrical analysis. Using C-AFM, we have demonstrated an analysis of the localized dielectric BD using topographical and current images. The lack of understanding on the physical analysis of these C-AFM induced BD is largely due to the several experimental difficulties involved in identifying the BD locations and isolating accurately after the C-AFM analysis to prepare the sample containing these extremely local BD locations for the physical analysis using TEM. Here, we present a technique to induce degradation and BD of the of a HfO2/SiOx dielectric stack locally using STM/SEM system [16], [17], in association with the nano-probing technique. The STM induced BD devices were identified and prepared the FIB sample containing BD spot for the physical analysis using TEM. Two devices were used for STM tip induced BD events. The first device was subjected to moderate BD (~2-3 orders of the initial leakage current) and the second device for hard BD (i.e. very high conductivity after the BD). Fig. 10 shows the tip placed at Au/Ti gate electrode area on the HfO2 dielectric. Figure 11. (a) Cross-sectional TEM micrograph of Au/Ti/HfO2/SiOx stack showing BD event for stressing moderate BD hardness. (b) TEM micrograph with high magnification and (c) STEM at the BD location indicated by dotted rectangle in (a). (d) Elemental mapping at the location highlighted by a dot at “ball-shaped” capping layer in (c) indicating Au migration to the Si substrate at the BD site [6]. Fig. 12(a) and Fig. 12(b) show the cross-sectional TEM of a non-BD and HBD devices, respectively. Fig. 12 (b) displays the catastrophic damage at the BD site with the complete rupture of the dielectric stack, melting and diffusion of gate electrode, and a burnt mark in Sisubstrate. The gate material melted with the creation of high local temperature at the BD site due to the thermal joule heating effect [18], [19]. Figure 10. SEM micrographs showing an STM tip placed on top of Au/Ti/ HfO2/SiOx stack. Figure 12. Cross-sectional TEM micrograph of (a) a non-BD location and (b) hard-BD location, showing catastrophic failure of Au/Ti/HfO2/SiOx stack. Rupture of HfO2/SiOx dielectric stack, Si substrate melting, gate electrode melting and diffusion were observed at the BD site. Fig. 11(a) shows the TEM micrograph of the stressed device containing the BD region (moderate BD). Fig. ©2014 Engineering and Technology Publishing 84 International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 IV. [11] G. Bersuker, J. Yum, L. Vandelli, et al., “Grain boundary-driven leakage path formation in HfO2 dielectrics,” Solid-State Electronics, vol. 65, pp. 146-150, 2011. [12] K. McKenna, A. Shluger, et al., “Grain boundary mediated leakage current in polycrystalline HfO2 films,” Microelectron. Eng., vol. 88, pp. 1272-1275, 2011. [13] K. Shubhakar, K. L. Pey, et al., “Grain boundary assisted degradation and breakdown study in cerium oxide gate dielectric using scanning tunneling microscopy,” Appl. Phys. Lett., vol. 98, pp. 072902(1-3), Feb. 2011. [14] N. Raghavan, K. L. Pey, K. Shubhakar, X. Wu, W. H. Liu, and M. Bosman, “Role of grain boundary percolative defects and localized trap generation on the reliability statistics of high-κ Gate dielectric stacks,” in Proc. IEEE International Reliability Physics Symposium (IRPS), 2012, pp. 6A. 1.1-6A. 1.11. [15] R. Ranjan, K. L. Pey, et al., “A comprehensive model for breakdown mechanism in HfO2 high-k gate stacks,” in Proc. IEEE International Electron Device Meeting (IEDM), 2004, pp. 725-728. [16] A. Kaneko, Y. Homma, H. Hibino, and T. Oginoc, “Ultrahigh vacuum scanning electron microscope system combined with wide-movable scanning tunneling microscope,” Rev. Sci. Instrum., vol. 76, pp. 083709 (1-9), Aug. 2005. [17] A. Wiessner, J. Kirschner, G. Schäfer, and T. Berghaus, “Design considerations and performance of a combined scanning tunnelling and scanning electron microscope,” Rev. Sci. Instrum., vol. 68, pp. 3790-3798, Jun. 1997. [18] R. Ranjan, K. L. Pey, et al., “Substrate injection induced ultrafast degradation in HfO2/TaN/TiN gate stack MOSFET,” in Proc. IEEE International Electron Devices Meeting (IEDM), 2004, pp. 1-4. [19] R. Ranjan, K. L. Pey, et al., “Breakdown-induced thermochemical reactions in HfO2 high-κ/polycrystalline silicon gate stacks,” Appl. Phys. Lett., vol. 87, pp. 242907 (1-3), Dec. 2005. SUMMARY An analysis on the degradation and breakdown phenomena was demonstrated at a very localized nanometer scale breakdown location in a HfO2/SiOx dielectric stack. Nanometer scale AFM analysis shows higher variation of localized electrical properties and morphology in polycrystalline HfO2. Therefore, the microstructure of the HK thin film plays a critical role in determining the TDDB robustness of advanced metal gate-HK stacks and process optimization to control the grain size and density distribution is bound to have a big effect on future CMOS performance and lifetime variability A combination of C-AFM and TEM can become an effective approach to understand the physical and electrical nature of failures in HK dielectric based MOS devices. ACKNOWLEDGEMENT This work is supported by Singapore University of Technology and Design (SUTD) Research Grant SRG ASPE 2010 004, NTU Research scholarship and SUTDInternational Design Centre (IDC) Research Grant IDG 11300103. REFERENCES Kalya Shubhakar received his Ph.D. (2013) from School of Electrical and Electronic Engineering, Nanyang Technological University (NTU), Singapore and M.Eng (2007) in Microelectronics (Electrical engineering Department) from Indian Institute of Science (IISc), Bangalore, India. He is currently working as a Senior Teaching Fellow in Engineering Product Development pillar at Singapore University of Technology and Design (SUTD), Singapore. His main research interests are in the nanoscale characterization and analysis of high-κ date dielectrics for logic and memory devices. He was a Graduate Student Member of IEEE (2010-2013). [1] K. L. Pey, R. Ranjan, C. H. Tung, L. J. Tang, W. H. Lin, and M. K. Radhakrishnan, “Gate dielectric degradation mechanism associated with DBIE evolution,” in Proc. IEEE International Reliability Physics Symposium (IRPS), 2004, pp. 117-121. [2] X. Li, C. H. Tung, K. L. Pey, and V. L. Lo, “The chemistry of gate dielectric breakdown,” in Proc. International Electron Devices Meeting (IEDM), 2008, pp. 779-782. [3] K. L. Pey, C. H. Tung, L. J. Tang, W. H. Lin, and M. K. Radhakrishnan, “Size difference in dielectric breakdown induced epitaxy in narrow n-and p-metal oxide semiconductor field effect transistors,” Appl. Phys. Lett., vol. 83, pp. 2940-2942, Oct. 2003. [4] K. L. Pey, R. Ranjan, C. H. Tung, L. J. Tang, W. H. Lin, and M. K. Radhakrishnan, “Breakdowns in high-κ gate stacks of nano-scale CMOS devices,” Microelectron. Eng., vol. 80, pp. 353-361, June 2005. [5] R. Ranjan, K. L. Pey, L. J. Tang, et al., “A new breakdown failure mechanism in HfO2 gate dielectrics,” in Proc. IEEE International Reliability Physics Symposium (IRPS), 2004, pp. 347-352. [6] K. Shubhakar, K. L. Pey, M. Bosman, R. Thamankar, et al., “Nanoscale physical analysis of localized breakdown events in HfO2/SiOx dielectric stacks: A correlation study of STM induced BD with C-AFM and TEM,” in Proc. IEEE International Symposium on the Physical and Failure Analysis of Integrated Circuits (IPFA), 2012, pp. 1-7. [7] K. Shubhakar, K. L. Pey, et al., “Study of preferential localized degradation and breakdown of HfO2/SiOx dielectric stacks at grain boundary sites of polycrystalline HfO2 dielectrics,” Microelectron. Eng., vol. 109, pp. 364-369, Sep. 2013. [8] M. Porti, S. Gerardin, M. Nafria, et al., “Systematic characterization of soft-and hard-breakdown spots using techniques with nanometer resolution,” Microelectron. Eng., vol. 84, pp. 1956-1959, 2007. [9] M. Lanza, K. Zhang, M. Porti, et al., “Grain boundaries as preferential sites for resistive switching in the HfO2 resistive random access memory structures,” App. Phys. Lett., vol. 100, no. 2, pp. 123508(1-4), 2012. [10] K. McKenna and A. Schluger, “The interaction of oxygen vacancies with grain boundaries in monoclinic HfO2,” App. Phys. Lett., vol. 95, pp. 222111(1-3), Dec. 2009. ©2014 Engineering and Technology Publishing Nagarajan Raghavan is currently pursuing his Post Doctoral Fellowship at the Singapore University of Technology and Design (SUTD). Prior to this, he was a PostDoctoral Fellow at the Interuniversity Microelectronics Center (IMEC) in joint association with the Katholieke Universiteit Leuven (KUL), Belgium. He obtained his Ph.D. (Electronics Engineering, 2012) at the Division of Microelectronics, Nanyang Technological University (NTU), Singapore and S.M. (Advanced Materials for Micro & Nano Systems, 2008) and M.Eng (Materials Science and Engineering, 2008) from National University of Singapore (NUS) and Massachusetts Institute of Technology (MIT), Boston respectively. His work focuses on statistical characterization and reliability modeling of dielectric breakdown in novel high-κ dielectric materials. His other research interests include random telegraph noise, prognostics for nanodevices, design for reliability and reliability statistics. Dr. Raghavan is the Asia-Pacific recipient for the IEEE EDS PhD Student Fellowship in 2011 and the IEEE Reliability Society Graduate Scholarship Award in 2008. To date, he has authored / co-authored around 80 international peer-reviewed publications and an invited book chapter as well. He is currently a Graduate Student Member of IEEE (2005-present) and invited member of the IEEE GOLD committee (2012-2014). 85 International Journal of Materials Science and Engineering Vol. 2, No. 2 December 2014 Kin Leong Pey received his Ph.D. (1994) in Electrical Engineering from the National University of Singapore (NUS). He is currently the Associate Provost (Education) at the Singapore University of Technology and Design (SUTD), Singapore and also holds a concurrent Fellowship appointment in the Singapore-MIT Alliance (SMA). He has held various research positions in the Institute of Microelectronics, Chartered Semiconductor Manufacturing (Global ©2014 Engineering and Technology Publishing Foundries®) and Agilent Technologies. In the past, he has served as a faculty member at the National University of Singapore and Nanyang Technological University (NTU) as the Head of Division for Microelectronics and Program Director of the Silicon Technology Research Group. His research interests include dielectric breakdown and interconnect reliability and failure analysis as well as design for reliability in integrated circuit and systems. He has published more than 170 international refereed publications and 175 technical papers at international meetings / conferences and holds 37 US patents. Prof. Pey is a senior member of IEEE and an IEEE EDS Distinguished Lecturer. 86
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