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Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse Surface plasmon polaritons THz emission Research Laboratory Course SPPs: jacopobertolotti.com/ Transfer tool at LMN

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Page 1: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

Deterministic transfer of h-BN/ graphene heterostructures for THz antennas

Sofía Cruces27.01.2021

fs laser pulse

Surface plasmon polaritons

THz emission

Research Laboratory Course

SPPs: jacopobertolotti.com/

Transfer tool at LMN

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S. Cruces Research Laboratory Course 2

Graphene and its conductivity

Anwar, et al. Digital Communications and Networks, 2018. 4(4), 244-257.

▪ Resonance condition: L=λSPP

2=

𝜋

𝑘𝑆𝑃𝑃

▪ Plasmon dispersion relation: 1

𝑘𝑆𝑃𝑃2−

𝜔2

𝑐2

+𝜀

𝑘𝑆𝑃𝑃2−𝜀

𝜔2

𝑐2

= −𝑖𝜎 ωμ𝑐τ

ωε0

→Challenge: high-quality graphene!

Chemical potential (𝛍𝐜)▪ Tuned by bias voltage or doping▪ Determines number of n & p in antennaRelaxation time (τ)▪ Average life time of charges▪ Determined by graphene quality

For functional antenna → large μ𝑐 & τ

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S. Cruces Research Laboratory Course 3

Structure of THz Antenna

+ -

50 μm

5 μm

200 μm

200 μm

Dipole antenna ▪ GaAs substrate (Eg = 1.42 eV)▪ Conduction lines & contact: Cr / Au▪ Two graphene patches

▪ Supports SPPs in THz band (0.1 – 10 THz)▪ Graphene SPP waves tuned by doping▪ Design/shape of graphene antennas

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S. Cruces Research Laboratory Course 4

Mechanical exfoliation

Freire Soler, Doctoral dissertation, 2014.

Advantages▪ Monocrystalline Graphene▪ Defect-free→ Cleanliness, high conductivity

Challenges▪ Low yield▪ Non-deterministic▪ Small and irregular flakes

Parameters:▪ Graphite source▪ Tape (Nitto, Tesa)▪ Force, speed, direction applied▪ Number of subsequent exfoliations

https://lmn.mb.uni-siegen.de/

Page 5: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 5

Challenges of mechanical exfoliation

50 μm

Nitto tape Tesa tape

Challenge → Residue removal

Residue

▪ Multiple subsequent exfoliations▪ 100 °C for 1 min→ Small, irregular & thick flakes

50 μm

Page 6: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 6

Tape residue removal

100 µm

Before acetone After acetone

100 µm

▪ 10 min in acetone▪ Blow dried with N2

→ Cleaner surface & flakes remain

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S. Cruces Research Laboratory Course 7

Exfoliation of large area graphene flakes

20 μm

▪ Less number of subsequent exfoliations▪ 75 °C for 3 min→ Clean, thin & bigger flakes

20 μm

Page 8: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 8

Thickness determination using contrast spectra

Novoselov, et al. Applied physics letters, 2007, 91(6), 063124.

▪ Model based on the Fresnel law▪ White light source and no filter

SiO2: 𝑛2(λ)= 1.47

Graphene: 𝑛1 = 2.6 – 1.3𝑖

Air: 𝑛0=1

𝑑1=0.34 nm

𝑑2=285 nm

Contrast equation

𝐶 =𝐼 𝑛1 = 1 − 𝐼(𝑛1)

𝐼(𝑛1 = 1)

Graphene

Substrate

Si: 𝑛3(λ)= 5.6 – 0.4i

Contrast of graphene on SiO2/Si

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S. Cruces Research Laboratory Course 9

Thickness determination using contrast spectra

Ni, et al. Nano letters, 2007, 7(9), 2758-2763.

𝐶 =𝐼 𝑛1 = 1 − 𝐼(𝑛1)

𝐼(𝑛1 = 1)

C = 0.0046 + 0.0925N − 0.00255𝑁2

20 μm

MLGTLG

4LG

▪ Intensities with ImageJ

Contrast equation

Number of layers

Page 10: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 10

▪ No D – peak (1350 cm-1) ▪ G´ band – single Lorentzian profile▪ FWHM 22.3 cm-1

▪ IG/IG´ (0.37)→ Typical values for defect-free, ME graphene

20 μm

▪ 532 nm laser▪ 1200 l/mm grating▪ 600 nm center wavelength

1400 1600 1800 2000 2200 2400 2600 2800

Inte

nsity (

arb

. units)

Raman shifts (cm-1)

GaAs-Gr-02

Fit peak

1589.92

2685.26

2466.65

G

G*

Raman spectroscopy

Page 11: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 11

All-dry transfer method: Transfer tool

PDMS

PC

Glass slide

flake

Page 12: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 12

Stamping Scheme

Preparation of graphene/hBN flakes

x/y

β

α

Visual control

Substrate temperature[40 °C – 200 °C ]

1

2

3

4

5

Quality control of flakes / flake search

Page 13: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 13

Pick up technique of flakes

PDMS

PC 5wt %

Glass slide

hBN

SiO240°C

PDMS

PC 5wt %

Glass slide

hBN

SiO2

Selection of h-BN flake on SiO2/Si substrate h-BN flake on stamp

200 μm 100 μm

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S. Cruces Research Laboratory Course 14

Challenges▪ PC coating would break▪ PDMS sticked to the substrate→Parameter optimization

PDMS

PC 5wt %

Glass slide

hBN

SiO2100°C

Graphene

PDMS

PC 5wt %

Glass slide

SiO2100°C

PDMS

PC 5wt %

Glass slide

SiO240°C

i. ii.

iii.

Drop-down

Pick-up20 μm

Pizzocchero, et al. Nature communications, 2016, 7(1), 1-10.

Selection of graphene on SiO2/Si substrate

Pick up technique of flakes

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S. Cruces Research Laboratory Course 15

▪ Extremely low contrast on GaAs

▪ Raman measurements required

▪ High contrast at contact with Au 1400 1600 1800 2000 2200 2400 2600 2800

Inte

nsity/ a.u

Raman shifts/ cm-1

Sample Si-GR01

Fitted plot

1601.66

2740.88

2459.17

Flake on antenna (Transfer OM)

PDMS

Glass slide

Flake

SiO270°C

200 μm

50 μm

100 μm

50 μm

Thin flake on PDMS

Visibility of graphene/graphite on GaAs substrate

Flake on antenna (Transfer OM)

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S. Cruces Research Laboratory Course 16

▪ Raman spectroscopy mapping

▪ Rapid optical thickness using contrast

▪ Correlation of contrast and thickness on GaAs

▪ Complimentary techniques (AFM)

▪ Correlation of contrast and thickness on PDMS

Outlook

Page 17: Deterministic transfer of h-BN/ graphene heterostructures ... · Deterministic transfer of h-BN/ graphene heterostructures for THz antennas Sofía Cruces 27.01.2021 fs laser pulse

S. Cruces Research Laboratory Course 17

Prof. Benjamin ButzM.Sc. Charles OgollaLMN group members

Prof. Peter Haring BolívarInstitute of High Frequency and Quantum Electronics

Prof. Mario AgioLaboratory of Nano-Optics

Acknowledgements