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Characterization @ Agrate Brianza is devoted to the study with advanced techniques of materials and devices for the microelectronic industry. The challenge is to quantitatively describe chemical, structural, optical and electrical properties of very thin films (a few nm thick) and surfaces/interfaces. Actions are undertaken with state of the art-last generation instrumentation also available in industrial laboratories and/or with advanced facilities especially designed or adapted in Agrate B. In particular, expertise is focused on Scanning probe techniques, X-ray diffraction, reflectivity and fluorescence, Time of Flight Secondary Ion Mass Spectrometry, Mössbauer spectroscopy, Raman, Electron Paramagnetic Resonance and X-ray Photoelectron Spectroscopies, Magnetotransport and Ellipsometry. Electrical characterization of devices is focusing on non-volatile memories, emerging devices for neuromorphic applications, MIM capacitors for analog applications, MOS structures and transistors, quasi-static and dynamic evaluation of single and multiple quantum dots devices in presence of microwaves and magnetic field. Interactions are strong with academic and industrial research centers devoted to microelectronics worldwide. The unit is located inside STMicroelectronics at Agrate B. All the instrumentation is situated in the same building. The access is limited and protected by STMicroelectronics rules of access. Research is facilitated by the presence of multiple instrumentation at the same site, by 24 hours/day regulated access, by the habit of the experienced researchers to work in multidisciplinary and international teams. Scientific collaboration is envisaged for all the characterization experiments. In particular cases, to be discussed and approved, commercial collaborations are also possible. Preliminary measurements, free of charge, may be encouraged.

Please don’t hesitate to contact Claudia Wiemer or people in charge of the different facilities.

Characterization is structured in the following domains: Structural and Chemical, Optical, Electrical and Magnetoelectrical, Hyperfine interactions Please consult the linked webpages for additional information.

 

Structural and Chemical Characterization

 

 

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Chemical Characterization

XRD,XRR, XRF

Contact persons: Claudia Wiemer, Alessio Lamperti

Two instruments are available

1

Techniques (instrument name) XRD and XRR (HRXRD IS2000)
Technical characteristics Goebel mirror monochromator, 4 circle goiniometer, scintillator and position sensitive detector, equipped with Anton Paar sample holder for measurements vs temperature (RT-1200°C) in N2 or air. All the geometries for diffraction and x-ray scattering are in principle possible.
Materials /devices  to be analysed Thin inorganic films from 2 nm to 1 mm (less experience for the study of organic materials)
Samples Size ranging from 1 mm2 to 8 inches, possibility to scan x and y with 1/100 mm step. Sample maximum 2x2 cm2 for in situ XRD vs T
Excellence Instrument developed within the framework of the European Project (ESQUI: 2001-20014, RTD project n. GRD1-1999-11097) with the specific purpose of advancing x-ray diffraction and x-ray reflectivity characterization for thin films for the microelectronic industry. The combination of a position sensitive and a scintillator detector allows the precise measurement of sample thickness by x-ray reflectivity and x-ray diffraction analysis with enhanced signal to noise ratio, reducing the acquisition time and enhancing sensitivity to ultra thin films. The Instrument was then commercialized by Italstructures (Riva del Garda). The use of this instrument and the refinement of the data is of particular relevance for the microelectronic industry, in particular since the era of high-k materials, it reveals the signature of crystallization in thicknesses that were only accessible by TEM.
Relevant publications

Wiemer C. et al., Thin Sol. Films. 450/1, 134-137 (2004)

Colombi P. et al, J. Appl. Cryst. 41, 143–152 (2008)

Lamperti A. et al., Journal of The Electrochemical Society, 158 (10) G221-G226 (2011)

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2

Techniques (instrument name) XRF, TXRF and XRR (HRXRD IS3000)
Technical characteristics Instrument equipped with a solid state detector and a scintillator, for the simultaneous detection of x-ray reflectivity and x-ray fluorescence
Materials /devices  to be analysed Any surface, particular of interest for the detection of contaminant and for the determination of stoichiometric ratio in thin films. Reveals elements with Z>Al
Samples Size ranging from 1cm2 to 2 inches
Excellence The instrument was especially designed to determine the chemical composition of thin films of ternary chalcogenide alloys for phase change memories applications in the framework of the European project Chemaph (EU IST Project # 027561, 2006-2008). The combined detection of x-ray fluorescence and specular reflectivity allows on one hand the precise alignment of the sample to enhance the total external reflection, and therefore the sensitivity, for very thin films, on the other to perform, in principle, depth profiling of the chemical composition. An upgraded version of Maud software, developed in 2015, allowed for this analysis.
Relevant publications

O. Salicio et al, Journal of Applied Physics 105 , 033520 1-6 (2009)

Massimo Longo et al., Nano Letters 12, 1509-1515 (2012)

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Structural and Chemical Characterization

Time of Flight Secondary Ion Mass Spectrometry (TOF SIMS)

Contact Persons: Michele Perego, Alessio Lamperti

Techniques (instrument name) TOF SIMS ION-TOF IV
Technical characteristics Dual beam analysis. Ga primary ion (analysis 50x50 um2). Cs and O2 sputtering ions Time of flight analyzer: mass resolution > 10000 Detection limit ppm-1% Depth resolution < 1 nm Lateral resolution > 50 nm
Materials /devices  to be analysed Thin dielectrics (oxide of transition metals and rare earths); Nanoclusters (P, SiO) in Si or SiO2; profile doping and element diffusion.
Samples Thin films and multilayers at the nanoscale (typically max 100-200 nm depth scale); sample dimension min. 5 mm x 5 mm, max 15 mm x 30 mm, typical 10 mm x 10 mm) Sample holder: max 12-14 samples 10 mm x 10 mm. 8” wafer possible on special holder upon request
Excellence Profile doping Contamination microanalysis CMOS compatibility Nanostructures and nanoclusters 2D materials Structure evolution upon different treatment (growth conditions, annealing, reactant, chemical environment) Interest also for biological or bio-inspired systems.
Relevant publications

Alessandro Molle, et al., Advanced Materials Interfaces (2016)

R. Lo Conte, et al., Physical Review B 91, 014433 1-9 (2015)

Michele Perego et al., Nanoscale 7, 14469–14475 (2015)

M. Mastromatteo et al., Journal of Materials Chemistry C, (2016)

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Structural and Chemical Characterization

X-ray photoelectron Spectroscopy (XPS)

Contact Persons: Alessio Lamperti, Michele Perego

Techniques (instrument name) XPS ESCA PHI 5600
Technical characteristics Al monochromatic source 7mm & 2mm filaments; max 8 sample holders carrousel; angle resolved possible; Energy resolution 0.1 eV
Materials /devices  to be analysed Thin dielectrics; Si nanoclusters; 2D materials.
Samples Thin films; depth resolution down to few nm unless ion sputtering analysis; 15 mm X 15 mm max dimensions. Typical 2 pieces 10 mm X 10 mm in 1 sample holder
Excellence band alignment; study on confined structures (nano-clusters, nanostructures, 2D materials)
Relevant publications

S. Vangelista, et al., Nanotechnology 27 (2016) 175703

Michele Perego, et al., Nanoscale 7, 14469–14475 (2015)

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Structural and Chemical Characterization

Scanning electron microscopy (SEM)

Contact Persons: Sabina Spiga

Techniques (instrument name) ZEISS Supra40 field emission scanning electron microscopy
Technical characteristics

High performance featuring the GEMINI® column.

-Schottky field emitter.

-Resolution 1.0 nm at 20 kV at WD = 2 mm

1.3 nm at 15 kV at WD = 2 mm

1.5 nm at 10 kV at WD = 2 mm

2.1 nm at 1 kV at WD = 2 mm

5.0 nm at 200 V at WD = 2 mm

-Acceleration Voltage Range: 0.1 - 30 kV

-Probe Current Range: 4 pA - 20 nA,

-Chamber Detectors: Everhart-Thornley SE-detector with optically coupled photomultiplier. CCD-camera with IR-illumination.

-In-lens Detector Type: High efficiency annular scintillator detector mounted in GEMINI® column with optically coupled photomultiplier.

Materials /devices  to be analysed Semiconductor, device, nanostructures (nanowires, nanodts,….)
Samples

Chamber dimension:  330 mm inner diameter and 270 mm height for large

Current sample holder for small samples (1x1 to 4x4 cm2), possible to take image also in wafers up to 4-6” but with limited stage motion

Sample holder for both plan and cross-section view

Excellence  
Relevant publications  

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Structural and Chemical Characterization

Scanning probes

Contact persons: Graziella Tallarida, Stefano Brivio

two instruments are available

1

Techniques (instrument name) Scanning probes in air: AFM, STM, MFM/EFM, SCFM, KPFM, TUNA
Technical characteristics Spatial resolution on the surface plane is few nm. Maximum scan range 100x100 micron2
Materials /devices  to be analysed Main expertise in investigating hard surfaces (semiconductors, metals and insulators, 2D-materials).
Samples it is possible to measure entire wafers up to 6”, as well as small pieces of any size. A sample navigator system allows to precisely locate the measurement area
Excellence Commercial equipment. It is equipped for performing conductive-AFM with high sensitivity and with double lock-in for Kelvin Probe Force Microscopy. Solid expertise has been developed in the investigation of the local electrical properties of materials for RERAM by conductive-AFM and KPFM
Relevant publications

Jacopo Frascaroli et al., ACS Nano 9 , 2518–2529 (2015)

S Brivio, et al., Nanotechnology, 25 385705 (2014)

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2

Techniques (instrument name) Scanning probes in UHV and at variable temperature (25-1200 K): AFM, STM, KPFM, BEEM
Technical characteristics Atomic resolution achievable in all the temperature range
Materials /devices  to be analysed Main expertise in the in situ investigation of the atomic arrangement of flat and prepared surfaces by STM and STS
Samples only small samples (12-14 mm side) can be measured
Excellence The scanning probe tool is commercial (Omicron) and is mounted in the UHV system that includes MBE growth facility and XPS. It has been extensively used for the characterization of silicene
Relevant publications

D. Chiappe, et al., Advanced Materials 24, 5088 (2012)

D. Chiappe, et. al., Adv. Mater., 26: 2096–2101 (2014)

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Optical Characterization

 

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Optical Characterization

Visible and UV Raman spectroscopy

Contact Persons: Alessandro Molle, Alessio Lamperti

Techniques (instrument name) Multiwavelength micro-Raman spectroscopy
Technical characteristics Excitation wavelength in the visible (488 nm, 514nm, 633 nm) and in the UV (364 nm), macroscopic map acquisition; Renishaw Invia Analyzer; Renishaw RM100 Analyzer
Materials /devices  to be analysed Silicon, 2D materials, silicene, transition metal dichalcogenides, phosphorene, Germanium, silicides
Samples Bulk, thin films, 2D materials (sample or support size up to several cm2
Excellence MicroRaman spectroscopy is mainly developed in our unit to discern: -local stress induced in silicon structures -number of sheets and atomic ordering in 2D materials (silicene, germanene, MoS2). The activity has recently been shared with international partners in the framework of a European FET project: 2D-nanolattices (http://www.2dnanolattices.eu/) and CNR grant – Laboratori Congiunti con Univ. Texas at Austin, USA, and CARIPLO-Regione Lombardia grant "CrystEL"
Relevant publications

F. Fabbri et al., Nat Comm. 7, 13044 (2016)

E. Cinquanta, et al., J. Phys. Chem. C 117, 16719 (2013)

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Optical Characterization

 

Spectroscopic Ellipsometry

 

Contact Person: Elena Cianci

Techniques (instrument name) M2000-F ellipsometer (J. A. Wollam sco, Inc.)
Technical characteristics 1-5 eV, fixed angle
Materials /devices  to be analysed High-k materials, thin films of dielectrics, thin metal films
Samples Thin films, mostly dielectrics, possibility to host up to 8 inches wafers
Excellence Thickness measurement, extraction of dielectric constants. Possible to be mounted on the ALD reactor for in-situ measurements during ALD growth
Relevant publications Luca Lamagna, et al., Chemistry of Materials 24, 1080-1090 (2012)

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Electrical and Magnetoelectrical Characterization

 

 

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Electrical and Magnetoelectrical Characterization

Set-ups for Pulsed and DC electrical testing of devices

Contact Persons: Sabina Spiga, Stefano Brivio

Techniques (instrument name)

The electrical lab for the device testing is equipped with  two 6” probe stations and related rack for DC and AC testing (setup1 and 2), and one cryogenic manipulator (setup3).  The instruments can be adapted if necessary to different setups

Setup1: Agilent B1500A Semiconductor Device Parameter Analyzer with fours SMU and High Voltage Semiconductor Pulse Generator Unit( B1525A-FG); Agilent 81110 Agilent Pulse Pattern generator, 1 GHz Agilent MSO6104A oscilloscope; custom switch board for pulsed setup

Setup2: HP 4140B pA meter, Agilent E4980 precision LCR meter, PerkInElmer7265 DSP Lock-in Amplifier, Agilent oscilloscope 54622A, Keithley 6430 SubFemto Amp Source Meter

Setup3: TTP-4 probe station (4K-400 K); Lakeshore331 temperature controller, Stanford Lock-in SR830 DSP Lock-in Amplifier; Boonton72B Capacitance Meter, HP 4284A LCR meter, HP 4140B  pA meter

Technical characteristics

Current-voltage (IV) measurement capabilities of spot, sweep, and pulse measurement in the range of 0.1 fA - 1 A / 0.5 µV - 200 V

AC capacitance measurement in multi frequency from 100 Hz to 2 MHz

Advanced pulsed IV capability, up to 40 V high voltage pulse forcing for non-volatile memory evaluation

Materials /devices  to be analysed

RRAM non volatile memory, MOS and MIM capacitors, transistors, test device on novel materials

Samples

Devices from 1x1 cm2 to 6” at room temperature, 2x2 cm2 for the TTP-4 probe station

Excellence

Several type of measurements available. Dedicated software developed in-house with Labview, custom interface switching boards

-Versatile characterization of RRAM and memristive devices, switching dynamics, endurance, retention

- Capacitance- voltage and current-voltage of MOS and MIM devices, as a function of temperature, low current measurements

- Transistor characterization

Relevant publications

S.Brivio et al., Appl. Phys. Lett. 107, 023504 (2015)  

S. Spiga et al.,  J. Appl. Phys. 112, 014107 ( 2012)

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Electrical and Magnetoelectrical Characterization

Internal Photoemission Spectroscopy (IPE)

Contact Person: Gabriele Seguini


Electrical and Magnetoelectrical Characterization

Quantum transport

Contact Persons: Marco De Michielis, Matteo Belli, Marco Fanciulli

Techniques (instrument name) Quantum transport measurements on semiconductor devices
Technical characteristics 12T Superconducting Cryomagnet 270mK Cryostat Technical characteristics Cryogenics 3He cryostat with base temperature down to 300 mK. Magnetic field up to 12 T. Possibility to transmit electric signals and microwaves toward the sample through a top-loading probe. Sensing of small electric signals due to a low noise cryogenic amplifier located on the probe shaft. Probe tip provided with a rotor for sample spatial orientation.
Materials /devices  to be analysed Quantum transport measurements on semiconductor devices. Expertise in the quasi-static and dynamic electrical characterization of single and multiple quantum dots devices in presence of microwaves and magnetic field.
Samples Typical measured devices are single and multiple quantum dot electrostatically and lithographically defined in the tens of nms size scale. Sample size compatible with a Dual In Line (DIL) socket.
Excellence The overall system is a commercial one with a custom probe that has been modified, during time, to host a low noise electronic amplifier. The system will be used in the H2020 ICT project (Grant Agreement n° 688539, MOS-QUITO). In this project, CMOS technology will be exploited to fabricate nanodevices to benchmark different architectures of quantum bits (qubits) based on spin states of confined electrons. The cryostat will provide the physical conditions (low temperature, EMR shielded environment, constant magnetic field) that, together with the probe performances (electrical interconnections with low parasitics) and with the low noise electronics, will let us perform initialization, manipulation and readout activities on one promising qubit architecture.
Relevant publications

M. L. V. Tagliaferri, et al. ,IEEE Transaction on Instrumentation and Measurements 65, 1827-1835 (2016)

E. Prati et al. Nanotechnology 23 215204, (2012)

G. Mazzeo et al., Applied Physics Letters 100 (21) 213107, (2012)

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Electrical and Magnetoelectrical Characterization

Magnetoresistance and Hall effect

Contact person: Roberto Mantovan

Techniques (instrument name) Magnetotransport
Technical characteristics Magnetotransport (5-300 K) up to 1.1 T at variable angles with respect to sample’s plane (0°-90°)
Materials /devices  to be analysed Hall: semiconductors, chalcogenides. MR: Ferromagnetic thin films (Fe3O4, Fe,..) and patterned structures (spin valves, Hall bars, magnetic
Samples Two sample holder available: 1. Up to 1 x 1 cm2 area for simultaneous rho, I-V, Hall, MR measurements in the Van der Pauw geometry and custom 2-point configurations (I-V, R, MR). Up to 4 x 8 mm2 samples with patterned structures to be bonded on chip
Excellence Close cycle cryostat, 24h measurements possible; home-built system for rotating the samples in the applied magnetic field; home-built LabVIEW-based software with possibility to run temperature-dependent simultaneous rho, I-V, Hall, MR measurements overnight/over the weekend
Relevant publications

R. Mantovan et al., J. Phys. D 43, 065002 (2010)

Roberto Fallica, et al., Applied Physics Letters 101, 102105 (2012)

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Hyperfine Interactions Methods:

 

 

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Hyperfine Interactions

57Fe and 119Sn Conversion electron Mössbauer spectroscopy (CEMS)

Contact person: Roberto Mantovan

Techniques (instrument name) Mössbauer Spectroscopy (MS): conversion electron-MS (CEMS) and emission-MS (eMS)
Technical characteristics Hyperfine interactions-based methods to conduct atomic-scale structural, chemical, magnetic studies in Fe, Sn-containing materials (lattice site, charge state, local symmetry/magnetism). Element-selective and non-destructive techniques.
Materials /devices  to be analysed CEMS: Sn, Fe -based thin films (Fe, Fe3O4, Fe3Si, Fe/oxides interfaces, Sn and Sn oxides,) eMS: Si, Ge, ZnO, TiO2, Al2O3, SnO2, dilute magnetic semiconductors/oxides, MnSi, MnGa, NiMnSn(In), nitrides, chalcogenides,… (in principle no limits), following their implantation with radioactive 57Mn/57Co/119In ions.
Samples CEMS: 1 x 1 cm2 thin films containing Fe and Sn. Typically 57Fe and 119Sn enriched samples are necessary, but in some systems (es: Fe3O4) also only with natural Fe if thickness ≥30 nm. eMS: 1 x 1 cm2 thin films (minimum thickness to valuate depending of implanted ion projected range in specific materials) and single crystals (max thickness: few mm)
Excellence CEMS: a dedicated parallel-plate avalanche counter (PPAC) operating from 295 K down to 100 K has been home-built in Agrate, and it is one of the few options for low temperature CEMS worldwide. When compared to standard lab. MS techniques, eMS is performed at extreme dopant dilution down to 10-4 at.%, being unique in providing atomic-scale probes to investigate materials in a regime of extreme dilution. Different custom-built sample mounting stages are available allowing to implant/measure in the 90-700 K temperature range, at variable angles, in 0.6T permanent magnetic field. Also quenching experiments are possible to get rid of implantation damage components. Researchers in Agrate B. have a long-standing experience in making use of the large-scale facility of ISOLDE at CERN to perform on line eMS in the framework of an international collaboration (http://e-ms.web.cern.ch/)
Relevant publications

A.Zenkevich et al., Appl. Phys. Lett. 99, 182905 (2011)

H.P. Gunnlaugsson et al.,  Appl. Phys. Lett. 97, 142501 (2010)

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Hyperfine Interactions

Electron paramagnetic Resonance Spectroscopy

Contact Persons: Matteo Belli, Marco Fanciulli

Techniques (instrument name) Electron Paramagnetic Resonance (Bruker Elexsys E580)
Technical characteristics Continuous wave and pulsed EPR in X-band and continuous wave EPR in Q-band in the temperature range from 4.2 K to 300 K.
Materials /devices  to be analysed Paramagnetic samples or samples containing paramagnetic centers.
Samples

X-band: ~1.2 cm x 3.5 mm; Q-band: 2-6 mm x 1.5-2 mm

X-band sample access: 4 mm, Q-band sample access: 3 mm).

Excellence The instrument is generally employed for the investigation of donors or defects in silicon and silicon nanostructures.
Relevant publications

M. Fanciulli et al., ECS Journal of Solid State Science and Technology 5, P3138 (2016)

M. Belli et al., Phys. Rev. B 89, 115207 (2014)

M. Belli et al., Phys. Rev. B 83, 235204 (2011)

M. Fanciulli et al., Phys. Rev. B 74, 134102 (2006)

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