CIM PACA Characterization Lab Materials Characterization - Failure Analysis

Presentation and description of facilities

April 2014

• Presentation of the lab

• List of equipment available through the lab

• Equipment descriptions

Contents

• The CIM PACA characterization lab is in the ROUSSET industrial park in the South of France

• It provides services in the following fields: – physico-chemical materials characterization – component failure analysis

• Services are provided to:

– current members of the association (Air Liquide Balazs – Aix Marseille University – Atmel – Biophy Research – IBS – Nexcis – Presto Engineering – Probion Analysis – STMicroelectronics – Tera Environnement)

– other non-members on request (external services)

• The facilities and equipment of the lab are operated by specialists from association members, which enables comprehensive service provision (including detailed analysis reports)

• The lab has been approved for French Research Tax Credits, which means that any R&D work is eligible for tax credits in France under this scheme

• For more information, please contact: Vincent GOUBIER - Operations Director Office line: +33 (0)4 42 68 51 60 – Mobile: +33 (0)6 47 23 84 75 E-mail: vincent.goubier@caracterisation.org Web: www.pf-caracterisation.org

Presentation

• FIB dual beam FEI Strata 400S

• FIB dual beam FEI Helios NanoLab 450S

• TEM FEI Titan 80-300

• TEM UHR FEI Cs-corrected Titan 80-300

• SEM Hitachi S-4800

• TEM specimen preparation NanoMill 1040

• Electrical test system Diamond D10

• Photon emission & laser scanning microscope Meridian WaferScan

• Time-resolved photon emission microscope EmiScope IIIt

• AFP nanoprober Multiprobe

• SEM-based nanoprober Kleindiek

• HR infrared thermography ELITE

• Laser ablation SESAME 1000

• Low-current test bench Cascade with Agilent instrumentation

• Electromigration test bench Aetrium

• Wafer tester Semilab WT-2000

Full list of equipment available at the lab

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• D-SIMS Cameca IMS 7f

• ToF-SIMS ION-TOF 5

• Micro AES PHI 700

• XPS Kratos Axis Nova

• Ellipsometer/GXR Sopra GES5-GXR

• 1D mechanical profiler Alpha-Step IQ

• 3D optical profiler Sensofar Neox

• AFM Veeco Dimension 3100 with SCM / SSRM / Extended-TUNA electrical modules

• Micro Raman (LabRAM HR800 coupled with a PSIA X100)

• VPD/ICP-MS IAS Expert / PerkinElmer NexION 300S

• ATD/GC/MS PerkinElmer

• Wafer Outgassing System PerkinElmer WOS 2000

• PTR/MS

• Organic contamination bench (permeation bench with reactor)

• Inorganic contamination bench

IMS 7f D-SIMS

• Secondary Ion Mass Spectrometry (SIMS) is a highly sensitive physico-chemical surface analysis technique. The sample surface is sputtered with a primary ion beam, eroding the surface and generating secondary ions, which are detected by the system.

• It can be used for elemental depth profile analysis (at micro- and nanoscale) on solids with a high level of sensitivity (parts per million or even billion, depending on the element). Analysis can be carried out on dopant distribution within silicon, for instance. D-SIMS is a destructive method.

• The minimum analysis size in terms of lateral resolution is of the order of 10*10 µm depending on the target concentration.

• Key features:

– Small sample size (approximately 7mm * 7mm)

– High mass resolution (separates 30SiH from P)

– Can be used on localised zones < 50µm2 (with reduced sensitivity)

– Good ultimate vacuum (Spec 7e-10mbar)

– Up to 500eV impact energy with O2+ (Shallow B)

– Up to 3keV impact energy with Cs- (As,P)

– Up to 500eV impact energy with Cs+

– Oxygen flooding can be used to reduce surface transient

TOF.SIMS 5 Time of Flight Secondary Ion Mass Spectrometer (ToF-SIMS)

• Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is based on static secondary ion emission. Unlike Dynamic SIMS (D-SIMS), which by nature erodes and deteriorates the sputtered surface, ToF-SIMS uses a total dose of primary ions of less than 1012 ions per cm² (just one primary ion for every 1000 surface atoms). ToF-SIMS is thus a soft ionisation technique for molecular analysis of a surface.

• The main application is highly sensitive elemental and molecular analysis of surface traces.

• A scanning beam of primary ions is used to map the various elements and molecular species present on the surface with a submicronic level of resolution.

• If the data acquisition process is coupled with an abrasion sequence, a composition profile can be plotted with a very high depth resolution.

PHI 700 micro-Auger (AES)

• Microscale Auger Electron Spectroscopy (Micro-AES) can be used for elemental surface analysis on solids (to depths of 0.5nm to 5nm) for elements at concentrations greater than 0.5% to 1%.

• The material is subjected to a beam of electrons and emits Auger electrons. The electrons emitted are counted (quantitative analysis) and their energy levels are measured to identify elements and chemical species).

• The Scanning Auger Microprobe uses a field effect electron gun and its argon ion source can be used to sputter surfaces for the purpose of depth profiling. The electron beam can be scanned to produce Auger chemical images.

• In some cases, the microprobe can give information about the bonding state of atoms (oxidised, metallic etc.).

• Lateral resolution is of the same order of magnitude as an SEM (particles ≥ 50nm).

AXIS Nova X-ray Photoelectron Spectroscopy (XPS)

• X-ray Photoelectron Spectroscopy (XPS) can be used to determine the chemical composition at the surface of any solid, to a depth of less than 10 nm. The material is irradiated with a beam of X-rays. The electrons emitted are counted (quantitative analysis) and their energy levels are measured to identify elements and chemical species.

• This information can be used to: – identify all elements present (except H) and determine their atomic concentration

(detection limit 1%) – determine the nature of bonds, the local environment and/or the degree of

oxidation of most of the elements – highlight any superficial segregation (angle-resolved analysis and/or ion beam

etching)

• The spatial resolution is 3µm in imaging mode and 10µm in microanalysis mode

• Depth profiling can also be carried out using a gradual etching process using an argon ion beam

GES5E-GXR Spectroscopic Ellipsometer (SE) and Grazing X-Ray Reflectometer (GXR)

• Spectroscopic ellipsometry (SE) and grazing X-ray reflectometry (GXR) are two techniques for determining the thicknesses of thin films.

• SE uses a broadband light source with a variable angle of incidence. The source makes it possible to characterise a sample within a range from 0.19µm (UV) to 2.05µm (near-IR). The complex reflection coefficients of the signal reflected by the sample can be analysed to give the n and k values for a film whose thickness is known or the thickness of a film whose optical properties are known.

• Grazing X-ray reflectometry (GXR) uses an X-ray incident beam. The variation in the intensity reflected back by the sample is measured as a function of the angle of incidence. This technique provides useful additional information alongside ellipsometry in measuring the thickness of film multilayers and can be used to determine surface and interface roughness values.

• Spot size: 60x40mm minimum in SE mode, approximately 1cm in GXR mode

• Non-destructive technique

Alpha-Step IQ 1D mechanical profiler

• A surface profiler is used to map surface topography in 1D, by running a stylus over the surface.

• Step heights from 10nm down to 2nm can be measured.

• The profiler is chiefly used to measure the depth of SIMS craters, which allows for depth calibration of the profiles.

PLµ neox 3D optical profiler

• This non-contact optical 3D profiler combine 3 non-destructive techniques in a single measuring head: confocal microscopy, interferometry et spectroscopic reflectometry.

• The instrument can therefore be used to analyze both rough surfaces (in confocal microscopy mode), smooth surfaces (in vertical scanning interferometry – VSI – mode) and very smooth surfaces (in phase-shifting interferometry – PSI – mode). Spectroscopic reflectometry mode allows transparent thin films measurement and analysis.

• The miscroscope is equipped with 6 objectives:

– Confocal objectives: 5X, 20X, 50X and 100X

– Interferometry objectives: 10X and 50X

• Key features:

– Vertical measurements: from 0.1nm to 40mm

– Vertical resolution: 0.1nm (in PSI mode)

– Lateral resolution: 0.2µm (in PSI or confocal mode)

– Transparent film measurements: thickness from 10nm to 20µm with a 0.1nm vertical resolution

Dimension 3100 Atomic Force Microscope (AFM)

• Atomic force microscopy is chiefly used to study the nanoscale topography of a surface (roughness etc.), but other electrical techniques derived from AFM (SCM, SSRM etc.) were subsequently developed (more details further on).

• A probing tips mounted on a micro-lever that reflects a laser beam is used to scan the sample surface. Tip deviation is measured by measuring the position of the reflected laser beam.

• AFM is a non-destructive technique.

• Vertical resolution is 0.75Å RMS (noise < 0.5 Å RMS). Lateral resolution is less than 5nm in tapping mode. Maximum amplitude is ±3µm. Maximum sample height is 20mm.

SCM module Scanning Capacitance Microscopy

• SCM is an AFM-derived electrical technique that also works by scanning a probe tip across a surface.

• SCM can be used to characterise surface implantations by measuring variations in the capacitance between the surface and the tip. Scanning can be carried out from above or using a cross-section.

• SCM is a non-destructive method.

• Lateral resolution is 15nm. The concentration range detected is from 1015 to 1020 at/cm3.

• A distinction can be made between n-type doping and p-type doping. SCM can highlight lightly doped zones with a high level of contrast and give a general view of heavily doped zones.

SSRM module Scanning Spreading Resistance Microscopy

• SSRM is an AFM-derived electrical technique that also works by scanning a probe tip across a surface.

• SSRM can be used to characterise surface implantations by measuring local resistivity variations in areas of the sample around the tip. Scanning can be carried out from above or using a cross-section.

• SSRM requires a high contact force between the diamond-coated tip and the sample. It is a destructive method.

• Lateral resolution is 10nm. The concentration range detected is from 1015 to 1020 at/cm3.

• The method does not distinguish between doping types (n-type and p-type). However can display heavily doped zones with a high level of contrast and give a general view of lightly doped zones. It can be used to separate out two levels of doping of the same type.

Extended-TUNA module TUNneling Atomic force microscopy

• Extended-TUNA is an AFM-derived electrical technique that also works by scanning a probe tip across a surface. The term covers two techniques: TUNA (TUNneling AFM) and C-AFM (Conductive AFM).

• Extended-TUNA can be used to characterise the uniformity of thin insulating films (maximum thickness 10nm). This module performs current imaging.

• Extended-TUNA scanning is carried out from above only.

• It is a non-destructive method.

• Lateral resolution is 15nm. The range of currents detected is in the tunnel current (60fA to 120pA) and "intermediate" current range (2pA to 1µA).

• Variations in resistivity between two zones can be highlighted; electrical faults and thin oxide breakdown can be located and analysed.

LabRAM HR800 (Raman spectrometer)

coupled with PSIA X100 (AFM) micro-Raman

• This unique system brings together vibrational spectroscopy with local probing microscopy

• The versatility of this set-up allows it to be used for in-situ studies on a wide variety of materials (semiconductors, insulators, polymers, molecular compounds etc.) without prior sample preparation

• The wavelengths available range from near-ultraviolet to near-infrared, including visible wavelengths

• Various different types of information can be gathered: composition, structure, stress, orientation, fluorescence, tomography etc.

• Analysis by main components and image reconstruction based on spectral information

VPD ExpertTM coupled with an ICP-MS NexIONTM300S VPD ICP-MS

• Vapor Phase Decomposition (VPD) coupled with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a physicochemical analysis technique which can be used to identify and quantify surface and volume concentrations of trace elements. The system includes a chemical decomposition and contaminants collection unit connected to a mass spectrometer.

• The technique allows analysis of either the surface or the volume of virgin silicon wafers or after cleaning, thin layers deposition, implantation or plasma treatment. Analysis of portions of the wafer surface is possible (rings, angular sectors, circles or squares), as well as wafer edge and wafer bevel . Moreover, contaminants collected by the VPD tool can be concentrated at the center of a virgin wafer to be analyzed by TXRF or ToF-SIMS.

• Key features:

– Samples : 6, 8 and 12-inch silicon wafers

– Films which can be analyzed : SiO2, SixNy , SiON, Poly-Si, c-Si

– Analyzed surface: from 2cm² to full wafer

– Volume analysis: 0.1mm depth (full wafer), 20mm depth (local)

– Detection limits: Variables depending on the element, the surface and/or the volume analyzed (from 1.10 7 to 5.10 9 at/cm² for surface or thin films analysis, from 1.10 12 to 1.10 14 at/cm3 for volume analysis in the silicon)

ATD GC MS PerkinElmer coupled with

WOS 2000 PerkinElmer

• By coupling gas chromatography (GC) and mass spectrometry (MS) with an Automated Thermal Desorber (ATD) sampling tubes system, tracesand ultra-traces of volatile organic compounds (VOCs) in the air can be identified and quantified

• These state-of-the-art techniques are used for monitoring the airborne molecular contamination (AMC) in the air of cleanrooms or enclosed environments

• The additional WOS (Wafer Outgassing System) is used to analysis wafer surface contamination, either as part of a specific process study, or after exposure of a 'control' wafer in the cleanroom

Strata 400S FIB dual beam

• This Dual-Beam FIB is a physical analysis system that can be used both to prepare and examine samples. The system features an ion beam for sample preparation (ion etching) and an electron beam (SEM) for in-situ examinations at a resolution of 2nm.

• This FIB is used to prepare lamella for transmission electron microscopy (in-situ sampling), with a high-precision locating function (some ten nm).

• The FIB is equipped with an STEM detector which allows acquisition of in-situ TEM-comparable images at a resolution of 1nm.

Helios NanoLabTM 450S FIB dual beam

• This version is equipped with a new generation of electron and ion columns in comparison to the equipment described on the previous slide, which gives the instrument exceptional performance levels for imaging, analysis, and TEM sample preparation.

• The innovative Elstar electron column with integrated monochromator provides high-resolution imaging capability (0.8 nm SEM and STEM resolution). The use of the beam deceleration mode permits to limit the charging effect and to obtain high-quality image on fragile materials such as resin (polymer).

• The Tomahawk ion column provides high-speed, high-resolution milling and cross sectioning (4.5 nm @ 30 kV). Its ability to maintain small beam diameter at less than 1 kV enables low-energy, grazing-incidence final clean-up to remove surface damage induced by higher-energy milling.

Titan 80-300 Transmission Electron Microscope (TEM)

• The TEM is a tool for physical characterisation of materials, which provides nanoscale morphological, structural and chemical information.

• Extremely small objects can be measured at resolution of 0.2nm (e.g. thickness of thin oxide layers <1nm) and the microstructure of thin films (grain size and orientation).

• The EDX analysis system can be used to determine the chemical composition of the analysed zone, with a probe size of less than one nanometre (e.g. to give concentration profiles through different layers of a sample).

» An Evactron RF Plasma Cleaner is available to decontaminate samples before inserting them into the TEM and examining them in HR STEM mode

Titan 80-300 Cs-corrected Ultra High Resolution Transmission Electron Microscope (UHR TEM)

• This version has 2 extra modules in addition to the equipment described on the previous slide, which gives the instrument exceptional performance levels for physico-chemical characterisation of materials:

– Image aberration corrector

– Electron energy loss spectroscope (EELS)

• The CS corrector means that objects can be measured with a resolution of less than 0.1nm

• The EELS module (GIF Tridiem with a 2K x 2K camera) can be used for electron structure and chemical composition analysis with spatial resolution that can be equivalent to the atomic column and an energy resolution of 0.7eV.

S-4800 Scanning Electron Microscope (SEM)

• This "semi in-lens" field emission SEM is optimised for high-resolution at low voltage and high voltage. It is the ideal scanning electron microscope for observing fragile materials such as polymers, semiconductors and in general for any studies relating to nanotechnologies.

• The system also features an energy dispersive X-ray spectrometer (EDX) for determining the chemical composition of the zone studied.

• Key features: – Resolution: 1.0nm at 15kV and 1.4nm at 1 kV – Cold field emission – Accelerating voltage: from 0.1 kV to 30 kV – Magnification range: x20 to x800,000 – Samples up to 200mm in diameter – "In-lens" SE and BSE detectors – STEM detector (Bright Field, Dark Field)

» A "high resolution" sputter coater (Emitech K575X) is available for

sample preparation prior to observation. It can be used to deposit very thin coats (secondary vacuum sputtering, Peltier-cooled coating, iridium target)

Diamond D10 digital tester

• This system can be used to confirm electrical diagnostics from the in-line test (i.e. electrical problems identified in the circuit being analysed).

• Signals are sent to the input pads:

– the signals are checked on the output pads (functional tests)

– power consumption is checked (Idd testing)

• The test system also aids in configuration of the integrated circuit by putting it in a steady state in order to find out the status of the transistors and locate any fault.

Meridian WaferScan photon emission & laser scanning microscope

• The Meridian is a tool that can identify failure zones in integrated circuits for the purpose of subsequent physical analysis.

• First of all, it is a static photon emission microscope (EMMI):

– It maps the transistors that emit photons and compares a failed IC with a properly-operating reference IC

– This can be used to determine which transistors are saturated and which are emitting photons abnormally

• The Meridian has also two laser beams : the first one heats the metal lines (OBIRCH technique) whereas the second one generates electron-hole pairs by photoelectric effect (OBIC technique). These lasers scan the circuit, causing variations in consumption when they pass over the critical points, which helps locate zones to be analyzed.

• The tool is equipped with a Solid Immersion Lens (SIL) which enables the highest optical resolution (up to 250nm) and sensitivity.

• LVI (Laser Voltage Imaging) and CW-LVP (Continuous Wave Laser Voltage Probing) techniques bring new opportunities in the failure analysis and allow to extend the analytical capability of the Meridian toward design debug:

– LVI shows the physical locations of transistors that are active at a specific frequency

– CW-LVP acquires functional waveform data

EmiScope IIIt time-resolved photon emission microscope

• This equipment is dedicated to dynamic analysis for functional failure analysis and design debug.

• We can monitor the light emission of a given transistor and how this emission evolves over a short period.

• Observing dynamic light emission and its occurrence in time provides in-silicon real timing data. This allows to check the proper functionality of transistors as well as providing accurate timing information.

• After analysis of these results, we can localize exactly the physical defect responsible for a functional defect or a timing issue.

Multiprobe AFP Atomic Force Prober (AFP)

Topographic image

Pico Current image

Ids vs. Vds curves

measurement

• This system allows electrical measurement probe tips to be nano-positioned for the probing of basic structures at the contacts or vias without using FIB and micro-machining the measurement points.

• There are 4 probing heads based on AFM (Atomic Force Microscopy) technology. The tips are mounted on micro-levers that reflect a laser beam and are used to scan the sample surface. The topographical image generated can then be used to position the tips on nanostructures on the sample.

• The prober is coupled with an HP4146 parametric analyzer for electrical characterisations.

• "PicoCurrent" mode: A fixed voltage is applied to the tip and a "PicoCurrent" imaging of the sample is generated by a scanning current measurement. This image can be used to detect junction or oxidation leakage and to differentiate contacts on type p or n implants.

• Key features: node size down to 65nm, contact pitch 200nm, positioning accuracy <10nm, noise <2nm, area scanned by each tip: 35µm*35µm, contact resistance <100Ω.

Kleindiek Prober Shuttle SEM-based nanoprober

• The Prober Shuttle is a tool for high-precision in-situ electrical probing. It offers low-current and low-capacity measurement capabilities.

• The Prober Shuttle is comprised of 4 ultra-flat three-axis high-stability and high-precision manipulators mounted on an ultra-flat two-axis substage. This 9mm-high system is installed in the SEM via the load-lock allowing a fast setup and removal.

• Probing can be done on metal lines (Cu, Al), as well as on W contacts and vias.

• The system enables :

– Electron Beam Induced Current (EBIC) analysis to locate irregularities in PN junctions

– Electron Beam Absorbed Current (EBAC) analysis to locate buried faults in metal lines and vias (shorts or opens)

• Key features:

– Maximum sample size: 25mm * 25mm * 1mm

– Low drift (probes): 1nm/min

– Sub-nanometer resolution: 0.25nm

– Low-current measurement: 1pA – 200mA

ELITE – Enhanced Lock-In Thermal Emission Infrared Thermography

• The ELITE is a tool that uses thermal detection to locate failures in integrated circuits in order to enable physical analysis of these zones. It can also be used for thermal mapping to validate design or to characterize behavior.

• The tool is capable of single die or stacked-die analysis as well as analyzing complete system cards or photovoltaic cells (localization of short-circuited cells because of a defective junction).

• The locating technique is non-destructive, with precision of the order of one micrometer and power dissipation sensitivity of the order of one microwatt.

SESAME 1000 laser ablation

• This tool has been designed for ablation of polymer or ceramic materials constituting the coating of electronic components. It allows precise package opening to carry out failure analysis. It can also be used for marking components in package.

• At the heart of the system is an Nd:YAG 1064nm diode-pumped laser. This wavelength is strongly absorbed by polymer material and very weakly by metals, enabling a selective removal. The laser beam diameter is around 50µm and can made very precise local openings of 300µm to several mm side.

• This technique is complementary to classic opening processes (chemistry). It enables use of less aggressive chemical opening techniques (at low temperature) for finishing.

Cascade Summit 12971B (prober)

Agilent 4156C / 41501B / E4980A (measurement) low-current test bench

• This system is used to determine the current-voltage and capacitance-voltage characteristic of semiconducting components (transistors, diodes, resistors, capacitors etc.).

• The set-up combines a Cascade semi-automatic prober and an Agilent analyzer.

• The prober characteristics enable measurements to a resolution of 1 fA (10-15 A).

• The temperature range for measurements is 0 to 200°C.

Aetrium® Model 1164 electromigration test bench

• This system is used for electromigration testing up to 350°C.

• It features 8 independent ovens for 8 parallel experiments. 16 samples per oven are electrically stressed in parallel.

• The samples are test structures that are inserted into 20 pin DIL-packages (16 packages per oven).

• Tests can last anything from a few hours to several weeks, depending on conditions.

• The current and temperature settings can be used for testing aluminium and copper technologies (at least down to 65nm).

• The purpose of this system is to enable process qualification: – 3 experiments can be run at the same current with different test temperatures (e.g. 250°C,

300°C, 350°C) to determine the metal activation energy – 3 experiments can be run at the same temperature but with different currents to determine the

current acceleration factor for the metal – the maximum current density that can flow through the metal cross-section can thus be

determined, with acceptable reliability criteria for the client

Semilab WT-2000 JPV, SPV, µ-PCD, Non-contact V-Q

• The techniques available on the Semilab WT-2000 apply only to silicon wafers (oxidised or otherwise) whose diameter is less than or equal to 200mm. The WT-2000 can be used to make maps, with a pitch adjustable from 62.5µm to 64mm.

• JPV: This tool allows contactless resistivity measurement for a substrate. The chief application is in mapping resistivity values after ion implantation and activation annealing.

• SPV/ µ-PCD

– The SPV tool measures the diffusion length of the minority carriers, which reflect the metallic contamination of the substrate. The volumetric concentration of iron after an activation process can be calculated from these measurements.

– The µ-PCD works in combination with the SPV tool and measures the lifetime of the minority carriers. The diffusion length is proportional to the square root of the lifetime.

– µ-PCD requires a surface passivation in order to eliminate the effects of surface recombination (e.g. iodine passivation). SPV requires a depleted surface (through corona charging).

• V-Q: This tool gives a contactless measurement of all parameters accessible by conventional C-V measurement: fixed, mobile and interface charge, electrical oxide thickness, flatband voltage etc.

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