The needs and challenges of electrical measurements for micro/nanoelectronic devices.

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1 The needs and challenges of electrical measurements for micro/nanoelectronic devices. Brice Gautier N. Baboux, D. Albertini, S. Martin, W. Hourani, A. Grandfond Institut des Nanotechnologies de Lyon Institut National des Sciences Appliquées de Lyon brice.gautier@insa-lyon.fr

Outline 2 Motivations : The needs in electrical measurements : why go nano? Existing tools : A wonderful tool which allows electrical measurement at the nanoscale : Techniques based on Atomic force microscopy : a short overview Some problems : Increasing the quality of electrical measurement at the nanoscale : where are the challenges? Overview of sources of errors in AFM based electrical measurements The area of contact The environment The signal to noise ratio Wish list for future improvements

Electrical measurements at the nanoscale : what for? 3 Social issue Calculation power Energy consumption Figures of merit Device Transistors Speed Reliability : failure analysis Energy yield Lifetime Memories Sensors Data storage Photovoltaic cells Measurement Retention time Fatigue Power Metrology Density of integration Accuracy, repeatability, trueness, reproducibility MEMS / NEMS Cost interconnexions

Electrical measurements at the nanoscale : how? 4 Near Field Microscopies : Electronic Microscopies A nanometric electrode positionned with a nanometric precision Scanning Electronic Microscopy (SEM) Photodiode Laser Transmission Electronic Microscopy (TEM) => Holographic TEM for dopant mapping => sample preparation! Spatially resolved Electronic spectroscopies : PEEM and derived methods => Work function measurement under UHV

Electrical measurements at the nanoscale : how? 5 Near Field Microscopies : Electronic Microscopies A nanometric electrode positionned with a nanometric precision Scanning Electronic Microscopy (SEM) Photodiode Laser Transmission Electronic Microscopy (TEM) => Holographic TEM for dopant mapping => sample preparation! Spatially resolved Electronic spectroscopies : PEEM and derived methods => Work function measurement under UHV

Atomic Force Microscopy 6 Contact mode : Tip in contact with sample High strain applied on the surface Act as a metallic electrode Silicon, metal-coated tips (PtIr5, diamond, CoCr...) Non-contact mode : Tip in oscillation above the sample No (little) strain applied on the surface Interaction modifies the frequency of oscillation

AFM modes for electric and magnetic measurements 7 Designed for topography but allows wide choice of electric modes EFM SCM PFM Contact SMM DART PFM Non-contact Electric field BE-PFM Capacitance Ferroelectricity C-AFM TUNA SSRM «resiscope» KFM ESM single pass KFM Ionic conduction double pass KFM AM - KFM FM - KFM MFM Resistance Surface potential Magnetisation

Why go nano? The exemple of micro/nanoelectronics 8 MOS cell RAM Memories, MOS and CMOS transistors ---------------- Gain space!, but with the same available power (or higher)! Oxide Source ++++++++++ Q Drain Substrate Q C = U Q : charge => available current I U : applied voltage P = U I Electrical power => Capacitance must be preserved in spite of the scaling : portable devices (phones, computers ) => Greatest areas => Smaller thicknesses e => Higher permittivity 14 nm Fully Depleted Silicon on Insulator (FDSOI) ϵs C = e Plane / Plane approximation Work faster! Increase frequencies of operation by reducing size The size of basic devices is of the order of several nanometers 3D FINFET

Overview of the characterization needs for the MOS gate 9 Gate and contacts Gate Properties under investigation : Oxide Source Work function : threshold voltage Vth shift Drain Substrate I ds Work function : threshold voltage shift (another challenge for the metrology of dimensions!) SEM view of the roughness on MOS transistor Court. J. JUSSOT, CEALETI V ds =50 mv Vt Vt' VG Resistivity Line Edge Roughness (LER) 1,7 nm desired, 4-5 nm achieved

Mesurement of work function with nanometric spatial resolution 10 Lift mode N. Gaillard, M. Gros-Jean, D. Mariolle, F. Bertin, A. Bsiesy, Appl. Phys. Lett. 2006 Vac Sample Measurement of V0 (surface potential) by the cancellation of F by adjusting VDC VDC Double pass (lift mode, to remove any interference from the topography) Simple pass (harmonics)

Overview of the characterization needs for the MOS oxide 11 Regardless of the geometry, always the same components : gate, oxide, source, drain Oxide Properties under investigation : Permittivity high-k materials Leakage currents Gate Charged defects in the volume and at the interfaces Oxide Source Drain Substrate C = Life-time : breakdown at low voltages (time dependent dielectric breakdown) Endurance: evolution of the electrical parameters when in use ϵs e Plane / Plane approximation Ageing : evolution of the electrical parameters when not in use (agressive environment) All require a description at the nanoscale, not (only) because the size of the object is small but also because the phenomenon to describe is active at the nanoscale!

Leakage currents in MOS structure 12 C = V ϵs e V Plane / Plane approximation SiO2 : less than 1 nm High-k materials (e.g. HfO2) Direct tunnel Fowler Nordheim = High leakage Higher Same capacitance Higher thickness Defects in the oxide volume => Poole Frenkel transport mechanisms Leakage currents => injection of defects in the oxide => ageing of the transistor => failure Percolation model J. Sune, IEEE trans. Electron. Dev. 22:392, 2001 Radius of the conducting channel in the nanometer range Dielectric breakdown is an intrinsically nanometric phenomenon

Detection of leakage currents : conducting AFM 13 TUNA (Tunneling AFM, linear amplifier) : 60 fa 100 pa C-AFM (Conductive AFM, linear amplifier) : 10 pa 1 A A SSRM : (Scanning Spreading Resistance Microscopy, logarithmic amplifier) => 1 ma Sample Resiscope : (logarithmic amplifier) : 100 fa 1 ma Leakage and breakdown : «Hot spots» in a dielectric layer LAO 3.5 nm Silicon Amorphous LaAlO3 (LAO), MBE, thickness = 3 nm atomic oxygen versus molecular oxygen on the density of oxygen vacancies / hot spots in very thin LAO Negative voltage applied on the substrate : dark areas indicate high currents (Positive voltage applied on the substrate : bright areas indicate high currents)

Overview of the characterization needs for the MOS source and drain 14 Source and drain Properties under investigation : Doping level Low resistivity of contact, high currents for such a small size = Gate Oxide Source Drain Substrate High levels of doping (> 1019 at/cm3) Degenerate semiconductors Need for : 2D measurement of the dopants concentration Precision < 4 % Spatial resolution ~ several nanometer Ease of use

Dopant mapping with an AFM : Scanning Capacitance Microscopy (SCM) 15 C Capacitance accumulation MOS depletion n type doping level #1 metal VDC oxyde Semiconductor C doping level #1 C doping level #2 p type doping level #2 VDC V p n The variation of CMOS is inversely proportionnal to the doping level. n p 4.5 m p n p SCM image of a sample containing pn junctions @ 0.125 Vdc p n Phase signal

Dopant mapping with an AFM : Scanning Spreading Resistance Microscopy (SSRM) 16 Rtip A Rts Measurement of the spreading resistance C-AFM with logarithmic amplifier Hard force required on silicon => hard tips, surface damage 0 Depth m 2 m SSRM profile of a staircase sample D-doped layer (Si:B), spacing 20 nm

Photovoltaïcs 17 Organic solar cells short-circuit current p-n junction with creation of electron-holes pair by interaction with light Donor and acceptor materials are intermixed with typical spacings of several nanometers Solar cell characteristics : Open circuit voltage and short-circuit current with nanometric spatial resolution => power and yield of the solar cell Open circuit voltage Carriers life-time All solar cells : Combine nanometric resolution with large samples (several centimeters) Illustrations : courtesy Roland Roche PhD thesis, IM2NP, 2014

Summary of the needs 18 Dopant concentrations : all electronic devices Work function : threshold voltage, ohmic/shottky contacts, open circuit voltage for PV Current : dielectric breakdown, ferroelectricity, thermo/pyro electricity Resistance of contacts Time resolved measurement (life time of carriers for PV) Capacitance : permittivity (high-k materials ), sensors... Electro-mechanical coupling (piezoelectricity) : MEMS / NEMS

Temporary conclusion 19 Tools exist. Their spatial resolution is indeed nanometric Their develoment is now mature They are wide spread in the labs What are their performances from a metrological point of view? 4.5 m p n n p p n p

20 The problems

Overview of the parameters hindering reliability of AFM based measurements 21 Coating of the tip Repeatability Shape of the tip Repeatability Parasitic capacitances : chip sample, tip sample, apex sample... Trueness, reproducibility Nature of the tip sample contact Tip sample area of contact Trueness Species present on the surface : e.g. water (polar solvant, containing ions) Trueness What happens if you apply a huge electric field? Electrochemistry? Field driven diffusion? What happens when current flows : Joule heating? Ctip Clever Accuracy Reproducibility Trueness Reproducibility Reaching metrological quality of measurements seems to be a tough task! Cchip

Instrumental Challenges : TUNA 22 Size of the tip / contact area? Radius of the tip : 10 100 nm depending on the coating Area of contact important to compare measurements A Sample PtIr5 coated tip Estimated radius : less than 2 nm in UHV. SiO2 3.5 nm Silicon Weibull statistics P. Delcroix et al. Microelectronic Engineering 88 (2011) 1376 1379 Estimated surface in UHV : 10 ± 6 nm2 Red and green points : measurements on know surfaces of contact (large electrodes) Image : nanoandmore + scale laws of Weibull statistics Image : nanoworld

Instrumental Challenges : TUNA 23 Size of the tip / contact area? Radius of the tip : 10 100 nm depending on the coating A Very small area of contact Sample PtIr5 coated tip Estimated radius : 13 nm in air. SiO2 3.5 nm Silicon Image : nanoandmore 10 SiO2 (5 nm) W. Hourani et al. (PhD thesis, INSA Lyon) Fowler Nordheim injection I (pa) tunnel FN (5 nm) SiO2 (3.5 nm) tunnel FN (3.5 nm) 1 0 1 2 3 4 5 6 Vpointe (V) 7 8 9 Image : nanoworld

Here comes the water meniscus 24 Measurement in air : A water meniscus is present at the tip apex Water is a (bad) conductor Water modifies the distribution of electric field lines Weeks et al., Langmuir 21, 8096 (2005) Water increases the size of the contact area Force applied on the surface (setpoint) Roughness of the surface Coating Ievlev et al. Appl. Phys. Lett. 104(9), 2014

Does environment play a role on the result of electrical measurement? 25 Obviously : Yes! Oxidation of the tip-coating Weeks et al., Langmuir 21, 8096 (2005) SiO2 3.5 nm Silicon RVS : ramped voltage stress In air : permanent degradation of the tip after 8 RVS Oxidation? No degradation @ 130 C (less water) may confirm oxidation Pt + nh20 -> PtOn + 2nH+ + 2neR. Arinero et al. J. Appl. Phys.110 (014304), 2011,

Influence of the environment on the electrical measurements 26 Obviously : Yes! OH + H + Oxidation and dégradation of the sample H2 O + H SiO2 OH H2 O Silicon Silicon V>0 on sample OH- versus H+ injection under high electric field surface degradation SiO2 Surface degradation after poling of a 3,5 nm thick SiO2 layer on Si H+ SiO2 H2 O Silicon Oxidation of the sample (V<0 on sample) oxidation W. Hourani et al, J. Vac. Sci. Technol. B 29, 01AA06, 2011 W. Hourani et al, Microelec. Reliability 51:2097, 2011

Instrumental challenges : SSRM 27 (SSRM : same problem with the exact area of contact) Rtip Rech + Rtip + Rcb + Rts > 1 k Rts Rtip ~ 1 k Rech What if Rech < 1 k? Rcb Rech : Spreading Resistance Measurement of extremely high doping levels? Modulation of the force applied to the sample in order to modulate the spreading resistance Schulze et al. Ultramicroscopy 161, 2016 A Rtip : resistance of the tip Rcb : resistance of back contact Rts : resistance of the contact between the tip and the sample Measurement of conductors? 2, 3 or 4 probes systems => resolution = tens of nanometers

Instrumental challenges : SCM 28 CS : 10-18 10-17 F CCHIP CS CLEVER Influence of topograhy on SCM signal Resonance curve of the SCM sensor CECH + CLEVER + CCHIP : ~ 5.10-13 F! (0,65 pf with our system) SCM signal extremely small due to very small area of contact Signal drops for high dopant concentrations Signal to noise ratio drops because of stray capacitance Variation of the sensitivity of the SCM sensor as a function of the position of the levier on the sample

Inversion of contrast in SCM 29 Errors in the determination of carrier type in case of worn tip (loss of metal coating) Inversions of contrast expected also when the quality of the top oxide is bad (SCM signal vs concentration not monotonous any more) How to grow a good quality oxide when dopant profile is needed? (Temperature of growth must be kept low) worn tip Bad oxide Depth ( m) SCM analyses of n-type staircases : SCM data of opposite sign compared to lower concentrations

Lowering the stray capacitance 30 Solutions to enhance the signal to noise ratio? Subtract the parasitic capacitance Estevez et al. Appl. Phys. Lett. 104, 083108 (2014) Subtract the displacement current due to stray capacitance in order to extract the information of interest. (e.g. polarisation switching current) Simon et al. Rev. Sci. Instr. 88, 023901 (2017) Increase frequency + impedance matching => Scanning Microwave Microscopy Huber et al, Rev. Sci. Instrum. 81, 113701, 2010 Estevez et al. Appl. Phys. Lett. 104, 083108 (2014) ID = C dv / dt Simon et al. Rev. Sci. Instr. 88, 023901 (2017)

Lowering the stray capacitance 31 Lower parasitic capacitance? Suppression of the lever and chip Shielding High aspect ratio tips Hydrophobic tips Piezoelectric detection of the deflexion => sensitivity! Replace all AFMs! Surface and tip at the same potential Non contact / tapping modes Mechanical behaviour? Coating? Full metal tips and Joule effect https://www.nanoandmore.com/afm-probe-ar10-nchr.html Wang et al. Nanotechnology 25, 405703, 2014

The needs : a summary 32 Calibration samples Capacitance and resistance Known metal => know work function Known, reproducible and «perfect» oxide : SiO2, microelectronics fabrication facilities => known permittivity = 3,9 Known semiconductor substrate (MIS) Capacitor MIS Oxide MIM Oxide Support from modelisation required Complex geometries including AFM tips Simulation of the field lines cross talk Estevez et al. Appl. Phys. Lett. 104, 083108 (2014)

The needs : a summary 33 Magic tips Conductive (metallic) Constant shape (no more coating loss) Good mechanical properties => predictible shape => modelling High aspect ratio if no instrumental evolution New instrumentation 2-or-more probes AFM instruments Low capacitance set-up (remove cantilever and chip) Combine instruments (e.g. SCM + SSRM => impedance measurement) Combine large samples with nanometric spatial resolution (arrays of tips?) Control of environment Remove water Find a compromise between ultra-high vacuum / controlled atmosphere Beware of material modification due to absence / presence of water

Prioritary 34 Thank you for your attention