CaracterizaciónCaracterización de superficies de ... · Jennifer Curtis et al., Langmuir, 29,...
61
La Solución a su medida ScienTec Ibérica Caracterización Caracterización de superficies de superficies por por SPM, SPM, Nanoindentación Nanoindentación y FESEM y FESEM F Javier Ledesma Herrera ScienTec Ibérica [email protected]
Transcript of CaracterizaciónCaracterización de superficies de ... · Jennifer Curtis et al., Langmuir, 29,...
La Solución a su medida
1
ScienTec Ibérica
CaracterizaciónCaracterización de superficiesde superficiesporpor SPM,SPM, NanoindentaciónNanoindentación y FESEMy FESEM
F Javier Ledesma HerreraScienTec Ibé[email protected]
La Solución a su medida
2
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
3
ScienTec Ibérica
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
La Solución a su medida
4
ScienTec Ibérica
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
La Solución a su medida
5
ScienTec Ibérica MicroMicro--NanoNano Tools: which one?Tools: which one?
ApplyApplyfilter tofilter totake outtake outwavinesswaviness
Waviness MapWaviness Map
Roughness MapRoughness Map
La Solución a su medida
6
ScienTec Ibérica
Focus on Advanced Microscopy
MicrocoordenatesOpticalMachine
SPM Microscopy
Nearfield Microscopy
FE-SEM Microscopy
AFM Microscopy
La Solución a su medida
7
ScienTec IbéricaKeeping a strong link to Materials science
Mechanical profilers
We also have some smallsTools for special app.
NanoindentorsNano UTM
La Solución a su medida
8
ScienTec Ibérica
TheThe mostmost completecomplete opticaloptical profiler lineprofiler line
Classical Interferometers
Digital Holographic Microscope Metrology Profilers
Transmission Interferometers
Confocal +interferometry(France only)
La Solución a su medida
9
ScienTec Ibérica
SPM: La técnicaSPM: La técnica
AGILENT AFMs
La Solución a su medida
10
ScienTec Ibérica
www.scientec.es
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….
La Solución a su medida
11
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
12
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
13
ScienTec Ibérica
www.scientec.es
ModeMode Resonantes:Resonantes: TappingTapping ModeMode , Non, Non ContactContact ModeMode
La Solución a su medida
14
ScienTec Ibérica
www.scientec.es
Mode Resonantes: Tapping Mode , NonContact Mode
La Solución a su medida
15
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
16
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
17
ScienTec Ibérica
www.scientec.es
MedidasMedidas ElectricasElectricas en contactoen contacto
La Solución a su medida
18
ScienTec Ibérica
www.scientec.es
MedidasMedidas ElectricasElectricas enen tappingtapping
La Solución a su medida
20
ScienTec Ibérica
www.scientec.es
SpectroscopiasSpectroscopias Curvas de FuerzaCurvas de Fuerza
La Solución a su medida
22
ScienTec Ibérica TREC™Topography & RECognition ImagingSystem
La Solución a su medida
23
ScienTec Ibérica
www.scientec.es
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)
La Solución a su medida
25
ScienTec Ibérica
AFM-STM
Environmental Control
La Solución a su medida
26
ScienTec Ibérica
AgilentAgilent´́s Unique Positions Unique Position
La Solución a su medida
27
ScienTec Ibérica
www.scientec.es
¿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
La Solución a su medida
28
ScienTec Ibérica
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
La Solución a su medida
29
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)
La Solución a su medida
30
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]
La Solución a su medida
31
ScienTec Ibérica
Electrochemistry Cell Detail
Electrochemistry Liquid Cell with and without electrodes
La Solución a su medida
32
ScienTec Ibérica
La Solución a su medida
33
ScienTec Ibérica
www.scientec.es
NEW Agilent 7500NEW Agilent 7500 benefitsbenefits
La Solución a su medida
36
ScienTec IbéricaNano-Observer AFM Microscope
Accesible AFM:Easy to make quality imagesEasy to buy
Ask for a demo!
La Solución a su medida
37
ScienTec Ibérica
www.scientec.es
NanoindentationNanoindentation
Hardness and Young’s modulusLoss modulus, friction coefficient.
AGILENT G200
La Solución a su medida
38
ScienTec Ibérica
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)
La Solución a su medida
39
ScienTec Ibérica
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?
La Solución a su medida
40
ScienTec Ibérica
La Solución a su medida
41
ScienTec Ibérica
www.scientec.es
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
La Solución a su medida
42
ScienTec Ibérica
www.scientec.es
Testing instrumentation: Nano IndenterTesting instrumentation: Nano Indenter ®®
Coil/magnet assembly
Leaf spring
Capacitance gauge
IndenterSample
Tipically we impose force (electromagnetically) andmeasure displacement (capacitively).
La Solución a su medida
43
ScienTec Ibérica
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
La Solución a su medida
44
ScienTec Ibérica
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°
La Solución a su medida
45
ScienTec Ibérica
November 17, 2008Page 45
Results
La Solución a su medida
46
ScienTec Ibérica
November 17, 2008Page 46
6
8
10
12
14
16
18
20
22
24
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300
Modulus (GPa)
Dis p lac ement In to Sur f ac e (nm)
M N
Results from Dynamic Indentation Testing
La Solución a su medida
47
ScienTec Ibérica
November 17, 2008Page 47
Thin Films and Coatings
6
8
10
12
14
16
18
20
22
24
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300
Modulus (GPa)
Displacement Into Surface (nm)
M N
0
1
2
3
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300
Hardness (GPa)
Displacement Into Surface (nm)
M N
La Solución a su medida
48
ScienTec Ibérica
www.scientec.es
Automatic modulus mappingAutomatic modulus mapping
La Solución a su medida
49
ScienTec Ibérica
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
La Solución a su medida
50
ScienTec Ibérica
www.scientec.es
Automated Indent and ScanAutomated Indent and Scan
La Solución a su medida
51
ScienTec Ibérica
Nanovision: accuracy of positioning
La Solución a su medida
52
ScienTec Ibérica
www.scientec.es
LowLow--VoltageVoltage FieldField--EmissionEmission Scanning ElectronScanning Electron MicroscopyMicroscopy… the Agilent… the Agilent 8500 Compact FE8500 Compact FE--SEMSEM
La Solución a su medida
53
ScienTec Ibérica
8500 FESEM SPECS
FE-SEM Microscopy
La Solución a su medida
54
ScienTec Ibérica
field-emissionelectron source
all-electrostaticlenses
quadrant detector –secondary e-, backscattered, topography
La Solución a su medida
55
ScienTec Ibérica
La Solución a su medida
56
ScienTec Ibérica
www.scientec.es
ChallengesChallenges in SEM Imaging ofin SEM Imaging of thin filmsthin films
La Solución a su medida
57
ScienTec Ibérica
www.scientec.es
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.
La Solución a su medida
58
ScienTec Ibérica
www.scientec.es
Wide Variety of BiomaterialsWide Variety of Biomaterials
Biomaterials Medical Devices
Agriculture
Brain Tissue
ParasiteE-Coli bacteria
La Solución a su medida
59
ScienTec Ibérica
www.scientec.es
Energy and Charge Sensitive MaterialsEnergy and Charge Sensitive Materials
Particle on Glass NaCl
Gypsum
Polymers
Si Nanowires
La Solución a su medida
60
ScienTec Ibérica
www.scientec.es
Nanotechnology MaterialsNanotechnology Materials-- Electronics & MEMSElectronics & MEMS
March 5, 2014Confidentiality Label
60
Integrated Circuits Resist
Resist
Single Crystal -6H-SiC
GaN NanowireCNT on Electrode
La Solución a su medida
61
ScienTec Ibérica
www.scientec.es
Thank You
Thanks to our partners :
Rufino Sanchez 8328290 Las Rozas– Madrid
Tel: 91-8429467Fax: [email protected]
www.scientec.es
