EFRI 2-DARE: 2D Crystals Formed by Activated Atomic Layer

Deposition

2015 REM Program

Can Known Etching and Exfoliation Techniques

Reliably Thin Down MoS2?
Sebastian O. 1
Manzo , Yiyang Gong2 and Thomas. N. Jackson3
1Department of Materials Science and Engineering and 2Department of Electrical Engineering, The Pennsylvania State University

Introduction f Methods Results Trial Gas Pressure (mT)

RIE Results
Gas Ratio
(%Ar, %NF3)
Power (W) Self-Bias (V) Time (min.) Results

1 Ar+NF3 200 10%, 90% 150 -22 4 complete removal

2 Ar+NF3 150 10%, 90% 137 -11 1 complete removal

Molybdenum disulfide is a direct bandgap Ultrasonic Exfoliation
semiconductor that exhibits high mobility, high Adhesive Tape Exfoliation Tape Exfoliation
Water IPA
3 Ar+NF3 150 50%, 50% 100 -11 1 complete removal

4 Ar+NF3 150 95%, 5% 18 -3 1 controlled etch

on/off ratio and robust mechanical properties [2] 5 Ar+NF3 150 95%, 5% 20 -3 1 no change
in its 2-D form. 2-D semiconducting materials Bulk MoS2 [2] Process, by which 6 Ar+NF3 150 95%, 5% 23 -3 3 complete removal

that represent the ultimate limit in thickness 2D MoS2

flakes were exfoliated. Etched flakes from Trial 4 using RIE
are desired so that transistor sizes can be Before After Before After
further minimized while maintaining good
electrostatic control. Consequently, MoS2 is Ultrasonic Exfoliation
regarded as one of the most promising [3]
Bath Sonicator Probe Sonicator
materials for future applications in display,
flexible and biomedical electronics.
[3] color optical images of 1L-15L MoS2 Conclusion
nanosheets on 90 nm SiO2/Si, scale bar is
5m. Images used to approximate thickness of Significant progress has been made in
our samples. As shown in figures above, tape identifying etches for thinning MoS2, but our
[1] etching methods were not able to consistently
exfoliation yielded more and thinner flakes.
etch our samples. Since tape exfoliation yielded
more and thinner flakes than ultrasonic, our
Sonication devices used to exfoliate MoS2. Wet Etching Results samples were produced using this method. Wet
Water and IPA were used as sonicating liquids. no change, non-uniform etch, complete removal etching proved to be unsuccessful in
Time consistently thinning the flakes; however, RIE
Acid Temperature C Result
(minutes) was able to etch the MoS2 easily. From our
Wet Etching Trial 1 HNO3 85 60 no change
HNO3 85 75 complete removal observations, RIE shows the most promise as a
HNO3 85 90 complete removal reliable etching recipe for MoS2. Therefore, it is
Trial 3 HNO3 85 60 no change
Wet etching set up HNO3 85 70 no change recommended that more research goes into the
[1] some potential applications for MoS2 in 68% HNO3, HNO3 85 80 no change effect of using different gas ratios and self
Trial 4 HNO3 70 60 no change
display, flexible and biomedical electronics 33-40% HCl used HNO3 70 60 no change biases. In addition, characterization utilizing an
HNO3 70 90 no change atomic force microscope would provide more
HNO3 70 140 no change
Trial 5 HCl 50 60 non-uniform change accurate flake thicknesses after each trial, giving
Trial 6 HCl RT 60 no change more insight on which parameters to adjust.
Objectives Reactive Ion Etching HCl
HCl
50
30
60
60
no change
no change

RIE System RIE Model Acknowledgements

Identify reproducible etching and exfoliation Trial 5
Samples after 50C HCl 1 hour wet etch. This project was made possible through the
techniques for MoS2
National Science Foundations Emerging
Frontiers in Research and Innovation (EFRI) for
Develop a slow wet etching recipe for MoS2
Before Two-Dimensional Atomic Layer Research and
that shows a high degree of control.
Ar and NF3 get ionized Engineering (2-DARE) program.
Different ratios
Develop a dry etching recipe that can because of electric field from
successfully etch MoS2 flakes layer-by-
of Ar and NF3
were used.
electrodes in chamber. After References
layer. Particles accelerate and
[1] Akinwande D. et al, Nature Communications,5 6678 (2014)
bombard sample. [2]Center for Solid State Physics at Institute of Physics Belgrade
[3]Li.H, et al., ACS Nano, (2013)

The Penn States EFRI 2-DARE: 2D Crystals Formed by Activated Atomic Layer Deposition REM is sponsored by the National Science Foundation (EFMA 1433378).