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CaracterizaciónCaracterización de superficiesde superficiesporpor SPM,SPM, NanoindentaciónNanoindentación y FESEMy FESEM
F Javier Ledesma HerreraScienTec Ibé[email protected]
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IndiceIndice
Presentación ScienTec – relación con Agilent
Microscopias SPM: AFM, STM, SNOM
Como funciona un AFM
Principal ventaja del AFM sobre otras técnicas de alta resolución
¿Cual es el mejor AFM?
Los AFMs de Agilent: características diferenciadoras
El nuevo Agilent 7500
Nanoindentacion: ¿Qué es?
Propiedades a medir
Compact FESEM : ventajas
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Metrology & Surface Analisis
Scientec a Nanosurface specialist
2006:Agilent buys Molecular ImagingScienTec was ww the best MI distributor2008 Agilent buys Nanoindentors to MTS2009 Agilent buys FESEM in 2009
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What do we understand by surface characterization?: AFM-STM-SPMNanoindentersFE-SEM
: Mechanical/ Optical Profilers
Holographic Optical Profilers
: SNOM/ Multiprobe AFM
: thin film measuring systems
: service and applications teams
: Tribometry & scracth equipment
Metrological Optical Profilers
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ScienTec Ibérica MicroMicro--NanoNano Tools: which one?Tools: which one?
ApplyApplyfilter tofilter totake outtake outwavinesswaviness
Waviness MapWaviness Map
Roughness MapRoughness Map
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Focus on Advanced Microscopy
MicrocoordenatesOpticalMachine
SPM Microscopy
Nearfield Microscopy
FE-SEM Microscopy
AFM Microscopy
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ScienTec IbéricaKeeping a strong link to Materials science
Mechanical profilers
We also have some smallsTools for special app.
NanoindentorsNano UTM
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TheThe mostmost completecomplete opticaloptical profiler lineprofiler line
Classical Interferometers
Digital Holographic Microscope Metrology Profilers
Transmission Interferometers
Confocal +interferometry(France only)
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SPM:SPM: ScanningScanning ProbeProbe MicroscopesMicroscopes
STM: the tip is metalic and we sensetunneling current (Scanning TunnelingMicroscopy) in a conductive sample
AFM: the tip is silicon and we sense force(Scanning Force Microscopy or AFM)
SNOM: the tip is a fiber we illuminate thesample detecting optically reflected light(Scanning NearField Optical Microscopy)
Sistema que rastrea (Scannea) en X,Yuna palanca (sensor o Probe)siguiendo la topografía de la muestra línea alíneaconstruyendo una imagen Microscópicacon resolución Nanométrica.
Letter Soup Microscopies:MFM; LFM; CSAFM; SRRM, NCAFM, ECAFM, TUNNA; SthM,EFM, PFM; KFM, AM_FM, PM-FM, ECSTM, ESCPM, TERS, TFM….
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HowHow itit worksworks??
While rastering the sample inplane with the X;Y piezos thetopography variation moves upand down the cantilever
The vertical movement of thecantilever is tracked by thelaser and photodiode
BUT THIS IS NOTENOUGH …..
We need to control the applied force with a FEEDBACK loop
Deflection reference value (SP) in contact mode
Amplutide reference value (SP) in intermitent mode (tapping , Non contact)
Applied Force in the range of 1 nN (resolution 0,1 nN)Deflection resolution: 0,1 nm (1 Å) =H2
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Scanning Tip finds step up and cantilever deflects
Deflection point value is higher that deflection set point value
Piezo Tube Responds To Restore Cantilever Deflection
TheThe Contact ModeContact Mode FeedbackFeedback--LoopLoop
Note: the secuence represent the piezo respond to comeback to the deflection setpoint of AFM operation
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ModeMode Resonantes:Resonantes: TappingTapping ModeMode , Non, Non ContactContact ModeMode
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Mode Resonantes: Tapping Mode , NonContact Mode
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IMAGEN y ESPECTROSCOPIA FUERZASIMAGEN y ESPECTROSCOPIA FUERZAS
As a contact Sensor (Spectroscopy)based on spring model Fc=Kc.Xc,Kc=0,01N/m; Xc= cantilever deflection= 1nm; Atomic Scale Forces (10 pN) +- 1pN
*Mechanical Properties (Curvas F-d)*Electrical Properties (Curvas I-V)
As a Microscope (imaging):High resolution imaging device (x,y,z) 0,1 nmOperates on air, liquidsConductive & non conductive samplesMetrology measurements in X; Y; Z
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No solo resolución nanométricaNo solo resolución nanométrica
La palanca es un sensor en el NanomundoTambién es una herramienta (nanodedo)Nos permite interaccionar con la muestra y medirfuerzas ( espectroscopía)Todo ello en condiciones controladas o reactivas (ejcorrosión)Propiedades nanomecánicas, electricas, quimicas,Podemos trabajar en líquidos, hacer electroquímica,en temperatura….
Aprovechemos la resolucion espacialde ese nanodedo o nanosensor
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MedidasMedidas ElectricasElectricas en contactoen contacto
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MedidasMedidas ElectricasElectricas enen tappingtapping
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SpectroscopiasSpectroscopias Curvas de FuerzaCurvas de Fuerza
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CreatingCreating Nano LisaNano Lisa byby TCNLTCNL
To make the nanoartwork, researchers usedAgielnt AFM with a thermal cantilever to doThermoChemical NanoLithography, or TCNL
10 µm
Fabricating Nanoscale Chemical Gradients with ThermoChemical NanoLithographyJennifer Curtis et al., Langmuir, 29, 8675, (2013)
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¿CUAL ES EL MEJOR AFM?¿CUAL ES EL MEJOR AFM?
EL AGILENT , of course,Sobre todo para:
Electroquímica y control ambiental
STM (moleculas orgánicas)
Medidas electricas: Kelvin, Resiscope,Scanning Microwave
Medidas en liquidos
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Since 1993 beyond air AFMAgilent AFM was found as Molecular imaging in 1993 byProf Stuart Lindsay and Dr Jing from Arizona State UniversityOriginal goal: to develop an AFM head to work in liquidsand under temperature and enviromental control
They designed a revolutionary head to prevent samplemodification or alteration by evaporation or oxidation
Today´s second generation AFM holds more than 40patents and all the muscle that Agilent is bringing tothe SPM industry
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ScienTec Ibérica Atomic Resolution STM(SScanning TTunneling MMicroscopy - for Conductive Samples)
Room Temp
120° Celsius
Monolayer of hexabenzocoroneneon HOPG(18 nm scan)
Monolayer of 2,8,14-trimethyl-5,11,17Triazatrinaphthylene on HOPG (20nm scan)
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ScienTec IbéricaHigh Resolution – Organic monolayers
STM image of a achiral oligo-p-phenylenevinylene derivative at the liquid-sold interface. Despite being achiral, this molecule self-assembles into chiral‘windmill’ structures. Surprisingly, the supramolecular ‘windmill’ rotation depends on the chirality of the solvent. [Emerging solvent-induced homochiralityupon confinement of achiral molecules against a solid surface, Nathalie Katsonis, Hong Xu, Robert M. Haak, Tibor Kudernac, Zeljko Tomovic, Subi George,Mark Van der Auweraer, Albert P. H. J. Schenning, E. W. Meijer, Ben L. Feringa, Steven De Feyter, Angew. Chem. Int. Ed., 2008, 47, 4997-5001]
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Electrochemistry Cell Detail
Electrochemistry Liquid Cell with and without electrodes
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NEW Agilent 7500NEW Agilent 7500 benefitsbenefits
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ScienTec IbéricaNano-Observer AFM Microscope
Accesible AFM:Easy to make quality imagesEasy to buy
Ask for a demo!
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NanoindentationNanoindentation
Hardness and Young’s modulusLoss modulus, friction coefficient.
AGILENT G200
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November 17, 2008Page 38
Why Nanoindentation?
– Limited amounts of material
– Complex material
– Unhomogenous, need for spatial resolution
– Small volumes of material
– Smaller loads
– Nanoindentation is easier to ‘perform’
Instrumented indentation gives us easily hardness (H)and Young’s modulus (E) (E)
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Static Mode:
Young’s modulus
Yield stress / Hardness
Dinamic Mode (Continous Stiffnes Mode) for:
Storage and loss modulus (polymers)
Fracture toughness
Stress exponent for creep
What Standard Mechanical Properties areMeasured using Nanoindentation?
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ForceForce RangeRange ComparationComparation
Macro testing – static loads of over 30 NewtonsMicro testing – static loads from 0.5N to 30NNano testing – static loads from 10mN to 0.5NUltra-Nano testing – static loads below 30-10mN
AFM operates below these ranges
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Testing instrumentation: Nano IndenterTesting instrumentation: Nano Indenter ®®
Coil/magnet assembly
Leaf spring
Capacitance gauge
IndenterSample
Tipically we impose force (electromagnetically) andmeasure displacement (capacitively).
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0
10
20
30
0 100 200 300 400 500 600
Load
(mN
)
Displacement (nm)
slope = S
ht
hc for = 0.75
Each load/unload curve is asingle Modulus point
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November 17, 2008Page 44
9.95
10
10.05
4.95 5 5.05
Nominal ForceExcitation Force
Load
(mN
)
Time (seconds)
Dynamic Indentation Testing
-2
-1
0
1
2
-1
-0.5
0
0.5
1
0 10 20 30 40 50
Exc
itatio
n fo
rce
(µN
)
Response displacem
ent (nm)
Time (milliseconds)
= 0°
= 90°
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November 17, 2008Page 46
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Modulus (GPa)
Dis p lac ement In to Sur f ac e (nm)
M N
Results from Dynamic Indentation Testing
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November 17, 2008Page 47
Thin Films and Coatings
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Modulus (GPa)
Displacement Into Surface (nm)
M N
0
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Hardness (GPa)
Displacement Into Surface (nm)
M N
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Automatic modulus mappingAutomatic modulus mapping
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Nanoindenter:3D imaging options
Survey Scanning: 3D images with the linearencoded positioning stage
Large scanning areas up to 500x500 microns
Repositoning with 100 nm resolution
Nanovision: ·3D images + precisenanopositioning (2 nm).
INSEM: the indentation head inside a SEM
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Automated Indent and ScanAutomated Indent and Scan
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LowLow--VoltageVoltage FieldField--EmissionEmission Scanning ElectronScanning Electron MicroscopyMicroscopy… the Agilent… the Agilent 8500 Compact FE8500 Compact FE--SEMSEM
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field-emissionelectron source
all-electrostaticlenses
quadrant detector –secondary e-, backscattered, topography
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ChallengesChallenges in SEM Imaging ofin SEM Imaging of thin filmsthin films
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SEM imaging of a Graphene FilmSEM imaging of a Graphene Film-- CVD (chemical vapor deposition) on Cu foilCVD (chemical vapor deposition) on Cu foil
The intensity profile along the yellow line displaying fourplateaus representingMono-, bi-, tri- and quadruple-layer graphene.
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Wide Variety of BiomaterialsWide Variety of Biomaterials
Biomaterials Medical Devices
Agriculture
Brain Tissue
ParasiteE-Coli bacteria
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Energy and Charge Sensitive MaterialsEnergy and Charge Sensitive Materials
Particle on Glass NaCl
Gypsum
Polymers
Si Nanowires
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Nanotechnology MaterialsNanotechnology Materials-- Electronics & MEMSElectronics & MEMS
March 5, 2014Confidentiality Label
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Integrated Circuits Resist
Resist
Single Crystal -6H-SiC
GaN NanowireCNT on Electrode
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Thank You
Thanks to our partners :
Rufino Sanchez 8328290 Las Rozas– Madrid
Tel: 91-8429467Fax: [email protected]
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