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© Using Nanoelectrical Solutions to expand the capability of AFM Dr. Peter De Wolf [email protected]

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  • ©

    Using Nanoelectrical Solutions to expand the capability of AFM Dr. Peter De Wolf [email protected]

    mailto:[email protected]

  • ©

    Atomic Force Microscopy (AFM)

    3/29/2018 2

    • Microscopy technique based on raster-scanning and small tip-sample force interactions

    • Resolution

  • © ©

    Electrical Property Measurements with AFM

    3/29/2018 3

    Conductivity & Resistivity: C-AFM, TUNA, SSRM

    Electric Fields, Charge: EFM, KPFM

    Surface Potential / Workfunction: KPFM

    Impedance: sMIM

    Carrier density: SCM, SSRM, sMIM

    Piezoelectric properties: PFM

    Other: Scanning Gate, Pyro-Electric AFM, Photoconductive AFM,…

    Bruker Webinar

  • © ©

    Electrical Property Measurements with AFM

    3/29/2018 4

    Carbon NTs (4x2 µm)

    Height

    TUNA Current

    InP nanowire (2x1 µm)

    KPFM Potential

    Height

    Si DMOSFET (1x0.7 µm)

    SCM dC/dV Height

    Capacitor references (60x40 µm)

    sMIM Capacitance Height

    Pt nanoparticles in solution

    Height

    TUNA Current

    SECM Current

    Bruker Webinar

  • © ©

    Imaging & Spectroscopy

    3/29/2018 5

    Height (nm) Current (pA) I-V Spectra

    +

    + +

    +

    +

    + +

    +

    Tunneling AFM (TUNA) on a carpet of ‘standing’ carbon nanotubes (1x1 µm scan)

    Bruker Webinar

  • © ©

    Expand the Capability on 3 levels:

    • Capture electrical spectra in every pixel

    • Correlate electrical & mechanical properties

    • Eliminate contact mode limitations, and expand to soft & fragile samples

    3/29/2018 6 Bruker Webinar

  • © ©

    Expand the Capability on 3 levels:

    • Capture electrical spectra in every pixel

    • Correlate electrical & mechanical properties

    • Eliminate contact mode limitations, and expand to soft & fragile samples

    3/29/2018 7

    PeakForce Tapping

    Height Adhesion Current

    PeakForce TUNA on P3HT:CNT blends (700x700 nm scan)

    Collaboration with Ph. Leclere, Uni Mons, Belgium See also: Nanoscale 4, no. 8 (2012), 2705.

    Bruker Webinar

  • © ©

    DataCubes

    3/29/2018 8 Bruker Webinar

  • © ©

    DataCubes Electrical Characterization Principle

    • Fast Force Volume imaging: a force-distance spectrum in every pixel

    • Insert a ‘hold segment’ (= ‘dwell time’) and perform an electrical measurement during the hold segment: electrical spectrum in every pixel

    3/29/2018 9

    DC Sample

    Voltage

    Electrical Channel

    Z Force

    Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Maghemite (γ-Fe2O3) • Force-distance & I-V spectrum in every

    pixel (110 ms/pixel)

    • TUNA current ‘slices’ shown as movie

    3/29/2018 10

    (movie)

    Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Maghemite (γ-Fe2O3) • The datacube can be analyzed as current ‘slice’ data

    • The datacube can be analyzed as I-V spectra

    3/29/2018 11 Bruker Webinar

  • © ©

    DataCubes Electrical Characterization Principle

    3/29/2018 12

    MECHANICAL

    Force Volume DCUBE-TUNA DCUBE-SSRM DCUBE-SCM DCUBE-sMIM DCUBE-PFM

    Ramp

    ParameterDistance VDC VDC

    VDC

    VAC

    fAC Phase

    VDC

    VAC

    fAC Phase

    VDC

    VAC

    fAC Phase

    Output

    Channel

    Force

    → Stiffness

    → Adhesion

    → Modulus

    Current log(Resistance)dC/dV Amplitude

    dC/dV Phase

    dC/dV Amplitude

    dC/dV Phase

    sMIM-C

    sMIM-R

    PFM Amplitude

    PFM Phase

    Example

    Spectra

    ELECTRICAL

    Bruker Webinar

  • © ©

    Capture electrical spectra in every pixel

    3/29/2018 13

    More information than other electrical AFM modes

    Access previously inaccessible material properties and device data

    Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Maghemite (γ-Fe2O3)

    3/29/2018 14

    𝑉𝑏+ = −ln(𝑎)

    𝑏 > 0

    Ohmic

    No Conduction

    • Using Matlab export/import functions, one can perform custom analysis: Here we fit all I-V spectra to extract potential barriers:

    • Data processing by N. Chevalier & D. Mariolle at Uni. Grenoble Alpes, CEA, LETI

    𝑦 = 𝑎𝑒𝑏𝑥 + 𝑐𝑒𝑑𝑥

    (movie)

    Bruker Webinar

  • © ©

    DCUBE-SCM (Scanning Capacitance Microscopy) on SRAM Transistors

    3/29/2018 15

    • Sample voltage ramp from -2V to 2V

    • 128x128 pixels, 2x2 µm scan

    • 100 ms/pixel (27 min/cube)

    • Data courtesy: N. Chevalier & D. Mariolle at Uni. Grenoble Alpes, CEA, LETI, France

    -1.6V -1.2V -0.8V -0.4V

    p n p p n p

    dC/dV Amplitude

    (movie)

    Bruker Webinar

  • © ©

    DCUBE-SCM (Scanning Capacitance Microscopy) on SRAM Transistors

    • Sample voltage (VDC) ramp from -2V to 2V in every pixel

    • Slices through the datacube show how the pnp junction profile changes with VDC

    • Data courtesy: N. Chevalier & D. Mariolle at Uni. Grenoble Alpes, CEA, LETI, France

    3/29/2018 16

    p n p

    p n p

    X

    Y

    Y

    VDC VDC

    slice at fixed VDC slice at fixed Y position

    dC/dV Amplitude DataCube

    Bruker Webinar

  • © ©

    DCUBE-sMIM (Microwave Impedance Microscopy) on Doped Si Device

    3/29/2018 17

    sMIM-C dC/dV Amplitude dC/dV Phase

    • C-V and dC/dV-V spectra (-2V to +2V) in every pixel

    -2.0V -1.5V -1.0V -0.5V 0.0V 0.5V 1.0V 1.5V 2.0V

    Bruker Webinar

  • © ©

    DCUBE-sMIM (Microwave Impedance Microscopy) on Si with staircase carrier profile

    3/29/2018 18

    • Sample voltage ramp from -2V to 2V in every pixel results in C-V spectra

    • Sample source: Infineon Munich, DOI: 10.1016/j.microrel.2014.07.024

    -1V

    +1V

    sMIM-R vs. time

    sMIM-C vs. time

    p-type n-type

    + +

    + +

    Bruker Webinar

  • © ©

    Practical Aspect: Speed?

    3/29/2018 19

    20 ms 100 ms 200 ms

    64x64 1.4 6.8 13.7

    128x128 5.5 27.3 54.6

    256x256 21.8 109.2 218.5

    Time per pixel

    Pixels

    Time per Image (min)

    200 ms

    100 ms

    50 ms

    25 ms

    12 ms

    sMIM C-V spectra on Si sample, collected at different speeds

    Typ. time (ms)

    Force-Distance Spectrum 10-100

    Electrical spectrum 10-100

    Total 20-200

    Mode Bandwidth (kHz)

    TUNA 15

    sMIM 300

    SCM 1-10

    PFM 1-10

    *fAC and LIA BW dependent

    Bruker Webinar

  • © ©

    DCUBE-PFM (Piezoresponse Force Microscopy) on BFO

    3/29/2018 20

    Amplitude

    Phase

    • PFM Amplitude and PFM Phase data slices

    • Domains switch as voltage is increased. Different domains switch at different voltages

    -6V -5V -4V -3V -2V -1V 0V

    Bruker Webinar

  • © ©

    DCUBE-PFM (Piezoresponse Force Microscopy) on BFO

    • Amplitude spectra along one line are shown

    • The images represent the PFM amplitude & phase vs. voltage along the line

    3/29/2018 21

    Sample

    Bias

    (V)

    X

    X

    0

    -1

    -2

    -3

    -4

    -5

    -6

    0

    -1

    -2

    -3

    -4

    -5

    -6

    Bruker Webinar

  • © ©

    Correlate electrical & mechanical properties

    3/29/2018 22 Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Battery Cathode

    3/29/2018 23

    • Modulus, Adhesion, Stiffness & conductivity from -4V to +4V

    • The data allow one to identify all elements (Li metal oxide, binder & carbon nanoparticles) and study differences between different metal oxide grains

    -3.5V -2.5V -1.5V -0.5V +0.25V

    +1V +1.75V +2.5V +3.25V +4V

    Carbon black

    Li metal-oxide

    Polymer binder

    Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Battery Cathode

    3/29/2018 24

    -500

    -100

    50

    200

    • Modulus, Adhesion, Stiffness & conductivity from -4V to +4V

    • All I-V spectra in selected area displayed

    +3V -3V

    Bruker Webinar

  • © ©

    DCUBE-sMIM (Microwave Impedance Microscopy) on Maghemite (γ-Fe2O3)

    3/29/2018 25

    • During a short hold segment, the DC bias was kept constant (no spectra)

    • Mechanical properties (Adhesion shown) acquired simultaneously

    • sMIM-C vs. time spectra shown for 5 positions

    sMIM-C sMIM-R

    Bruker Webinar

  • © ©

    DCUBE-CR-PFM (Contact Resonance PFM) on LiTaO3

    3/29/2018 26

    (movie)

    Bruker Webinar

  • © ©

    Eliminate contact mode limitations

    3/29/2018 27

    Longer tip lifetime

    Characterize soft & fragile samples

    Better spatial resolution

    Bruker Webinar

  • © ©

    DCUBE-TUNA (Tunneling AFM) on Battery Cathode

    3/29/2018 28

    -4.0V -3.0V -1.0V

    +1V +2.0V +3.0V +4.0V

    Bruker Webinar

  • © ©

    Peakforce-TUNA (Tunneling AFM) on P3HT Organic conductive nanowires

    3/29/2018 29

    • +3V sample voltage, 3x3 µm scan

    Height (nm) Adhesion (nN) Current (pA)

    Bruker Webinar

  • © ©

    Summary

    Combining Fast Force Volume imaging with Electrical modes generates Datacubes – enhancing the capabilities of conventional electrical AFM modes:

    • Capture electrical spectra in every pixel

    • Correlate electrical & mechanical properties

    • Eliminate contact mode limitations & expand to soft & fragile samples

    3/29/2018 30

    Height Modulus Current

    (movie)

    Bruker Webinar

  • ©

    © Copyright Bruker Corporation. All rights reserved.

    www.bruker.com

    © Copyright Bruker Corporation. All rights reserved.


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