ScienTec Ibérica. La Solución a su medida. F Javier Ledesma Herrera ScienTec Ibérica

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1 Caracterización de superficies por SPM, Nanoindentación y FESEM F Javier Ledesma Herrera ScienTec Ibérica j.ledesma@scientec.es 1

2 Indice 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 2

3 Scientec a Nanosurface specialist Metrology & Surface Analisis 2006:Agilent buys Molecular Imaging ScienTec was ww the best MI distributor 2008 Agilent buys Nanoindentors to MTS 2009 Agilent buys FESEM in

4 What do we understand by surface characterization? : AFM-STM-SPM Nanoindenters FE-SEM : Mechanical/ Optical Profilers Holographic Optical Profilers Metrological Optical Profilers : Tribometry & scracth equipment : SNOM/ Multiprobe AFM : thin film measuring systems : service and applications teams 4

5 Micro-Nano Tools: which one? Waviness Map Apply filter to take out waviness Roughness Map 5

6 Focus on Advanced Microscopy Microcoordenates Optical Machine FE-SEM Microscopy SPM Microscopy AFM Microscopy Nearfield Microscopy 6

7 Keeping a strong link to Materials science Mechanical profilers Nano UTM Nanoindentors We also have some smalls Tools for special app. 7

8 The most complete optical profiler line Confocal +interferometry (France only) Classical Interferometers Transmission Interferometers Digital Holographic Microscope Metrology Profilers 8

9 SPM: La técnica AGILENT AFMs 9

SPM: Scanning Probe Microscopes Sistema que rastrea (Scannea) en X,Y una palanca (sensor o Probe) siguiendo la topografía de la muestra línea a líneaconstruyendo una imagen Microscópica con

10 SPM: Scanning Probe Microscopes Sistema que rastrea (Scannea) en X,Y una palanca (sensor o Probe) siguiendo la topografía de la muestra línea a líneaconstruyendo una imagen Microscópica con resolución Nanométrica. STM: the tip is metalic and we sense tunneling current (Scanning Tunneling Microscopy) 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 the sample detecting optically reflected light (Scanning NearField Optical Microscopy) Letter Soup Microscopies: MFM; LFM; CSAFM; SRRM, NCAFM, ECAFM, TUNNA; SthM, EFM, PFM; KFM, AM_FM, PM-FM, ECSTM, ESCPM, TERS, TFM. 10

movement of the cantilever is tracked by the laser and photodiode BUT THIS IS NOT ENOUGH.

11 How it works? While rastering the sample in plane with the X;Y piezos the topography variation moves up and down the cantilever The vertical movement of the cantilever is tracked by the laser and photodiode BUT THIS IS NOT ENOUGH.. 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) =H 2 11

The Contact Mode Feedback-Loop Scanning Tip finds step up and cantilever deflects Deflection point value is higher that deflection set point value Piezo

12 The Contact Mode Feedback-Loop 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 Note: the secuence represent the piezo respond to come back to the deflection setpoint of AFM operation 12

13 Mode Resonantes: Tapping Mode, Non Contact Mode 13

14 Mode Resonantes: Tapping Mode, Non Contact Mode 14

IMAGEN y ESPECTROSCOPIA FUERZAS As a Microscope (imaging): High

Conductive & non conductive samples Metrology measurements in X; Y; Z

Xc, Kc=0,01N/m; Xc= cantilever deflection= 1nm; Atomic Scale Forces

15 IMAGEN y ESPECTROSCOPIA FUERZAS As a Microscope (imaging): High resolution imaging device (x,y,z) 0,1 nm Operates on air, liquids Conductive & non conductive samples Metrology measurements in X; Y; Z 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) 15

16 No solo resolución nanométrica La palanca es un sensor en el Nanomundo También es una herramienta (nanodedo) Nos permite interaccionar con la muestra y medir fuerzas ( espectroscopía) Todo ello en condiciones controladas o reactivas (ej corrosión) Propiedades nanomecánicas, electricas, quimicas, Podemos trabajar en líquidos, hacer electroquímica, en temperatura. Aprovechemos la resolucion espacial de ese nanodedo o nanosensor 16

17 Medidas Electricas en contacto 17

18 Medidas Electricas en tapping 18

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20 Spectroscopias Curvas de Fuerza 20

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22 TREC Topography & RECognition Imaging System 22

, Langmuir, 29, 8675, (2013) To make the nanoartwork, researchers used

23 Creating Nano Lisa by TCNL 10 µm Fabricating Nanoscale Chemical Gradients with Thermo Chemical NanoLithography Jennifer Curtis et al., Langmuir, 29, 8675, (2013) To make the nanoartwork, researchers used Agielnt AFM with a thermal cantilever to do ThermoChemical NanoLithography, or TCNL 23

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25 AFM-STM Environmental Control 25

26 Agilent s Unique Position 26

27 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 27

Since 1993 beyond air AFM Agilent AFM was found as Molecular imaging in 1993 by Prof Stuart Lindsay and Dr Jing from Arizona State University Original goal: to develop an AFM head to work in liquids

28 Since 1993 beyond air AFM Agilent AFM was found as Molecular imaging in 1993 by Prof Stuart Lindsay and Dr Jing from Arizona State University Original goal: to develop an AFM head to work in liquids and under temperature and enviromental control They designed a revolutionary head to prevent sample modification or alteration by evaporation or oxidation Today s second generation AFM holds more than 40 patents and all the muscle that Agilent is bringing to the SPM industry 28

hexabenzocoronene on HOPG(18 nm scan) Monolayer of

29 Atomic Resolution STM (Scanning Tunneling Microscopy - for Conductive Samples) Room Temp 120 Celsius Monolayer of hexabenzocoronene on HOPG(18 nm scan) Monolayer of 2,8,14-trimethyl-5,11,17 Triazatrinaphthylene on HOPG (20nm scan) 29

30 High 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 homochirality upon 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, ] 30

31 Electrochemistry Cell Detail Electrochemistry Liquid Cell with and without electrodes 31

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33 NEW Agilent 7500 benefits 33

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36 Nano-Observer AFM Microscope Accesible AFM: Easy to make quality images Easy to buy Ask for a demo! 36

37 Nanoindentation AGILENT G200 Hardness and Young s modulus Loss modulus, friction coefficient. 37

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) Page 38 November 17,

39 What Standard Mechanical Properties are Measured using Nanoindentation? 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 39

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41 Force Range Comparation Macro testing static loads of over 30 Newtons Micro testing static loads from 0.5N to 30N Nano testing static loads from 10mN to 0.5N Ultra-Nano testing static loads below 30-10mN AFM operates below these ranges 41

42 Testing instrumentation: Nano Indenter Coil/magnet assembly Leaf spring Capacitance gauge Indenter Sample Tipically we impose force (electromagnetically) and measure displacement (capacitively). 42

43 Each load/unload curve is a single Modulus point Load (mn) h c for = 0.75 slope = S h t Displacement (nm) 43

44 Dynamic Indentation Testing Nominal Force Excitation Force Load (mn) Time (seconds) Excitation force (µn) = 0 = Time (milliseconds) Response displacement (nm) Page 44 November 17,

45 Results Page 45 November 17,

46 Results from Dynamic Indentation Testing Modulus (GPa) M N Displacement Into Surface (nm) Page 46 November 17,

47 Thin Films and Coatings Modulus (GPa) 24 Hardness (GPa) M N 10 8 M N Displacement Into Surface (nm) Displacement Into Surface (nm) Page 47 November 17,

48 Automatic modulus mapping 48

49 Nanoindenter:3D imaging options Survey Scanning: 3D images with the linear encoded positioning stage Large scanning areas up to 500x500 microns Repositoning with 100 nm resolution Nanovision: 3D images + precise nanopositioning (2 nm). INSEM: the indentation head inside a SEM 49

50 Automated Indent and Scan 50

51 Nanovision: accuracy of positioning 51

52 Low-Voltage Field-Emission Scanning Electron Microscopy the Agilent 8500 Compact FE-SEM 52

53 8500 FESEM SPECS FE-SEM Microscopy 53

54 all-electrostatic lenses field-emission electron source quadrant detector secondary e -, backscattered, topography 54

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56 Challenges in SEM Imaging of thin films 56

57 SEM imaging of a Graphene Film - CVD (chemical vapor deposition) on Cu foil The intensity profile along the yellow line displaying four plateaus representing Mono-, bi-, tri- and quadruple-layer graphene. 57

58 Wide Variety of Biomaterials Brain Tissue Biomaterials Medical Devices E-Coli bacteria Parasite Agriculture 58

59 Energy and Charge Sensitive Materials Particle on Glass Polymers NaCl Si Nanowires Gypsum 59

60 Nanotechnology Materials- Electronics & MEMS CNT on Electrode GaN Nanowire Resist Integrated Circuits Single Crystal -6H-SiC Resist 60 Confidentiality Label March 5,

61 Thank You Rufino Sanchez Las Rozas Madrid Tel: Fax: Thanks to our partners : 61

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