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MitgliedderHelmholtz-Gemeinschaft
2009 iNNIN REU
Electrochemical Deposition of Polyaniline on
Nanoelectrode CrossBar Structures
José Guevarra
Department of Mechanical Engineering
University of California, Santa Barbara
PI: Dr Dirk Mayer
Mentor: Nils Sanetra
29. Januar 2015 Folie 2
Outline
• Motivation
Molecular bioelectronics
• The crossbar structure
• Polyaniline (PANI)
• Goals
• Methods
• Crossbar Structure Fabrication
• Electrochemical deposition of PANI on Au
• Summary and Outlook
• Acknowledgments
29. Januar 2015 Folie 3
Molecular electronics
What is molecular bioelectronics?
• Miniaturization
• Alternative to CMOS
Bioelectronics
• Biomolecule as active part
• Totally new functions (e.g.
sensor)
29. Januar 2015 Folie 4
The crossbar architecture
What is a crossbar?
• Two parallel planes of
nanoscale wire arrays
• Propterties of the crossbar
determined by interjunction
layer
• Metal-Bridge-Metal (MBM)
• For bioelectronics:
Interjunctionlayer: SAM
[Snider et al 2005]
29. Januar 2015 Folie 5
Polyaniline (PANI)
• Well documented conducting polymer
• Can be acid-doped to form conducting salt (emeraldine)
• Can be electrochemically deposited
• Cheap
Can it be used to close the interjunction gap?
29. Januar 2015 Folie 6
Goals
• Fabricate crossbar structures using a soft mold and lift-off
process
• Characterize pattern fidelity and compare to other methods
• Electrochemically deposit a conducting polymer (Polyanaline)
to bridge the junction gaps between crossbar junctions
• Electronic characterization of polyaniline, electrodes, and
junctions
29. Januar 2015 Folie 7
Methods
29. Januar 2015 Folie 8
Crossbar Structure Fabrication
29. Januar 2015 Folie 9
Fabrication Process (NanoImprint Lithography)
CF4 Etch
O2 Etch
Gold Deposition
Lift-Off
Using a soft mold (Surlyn) allows one to imprint a pattern from a
rigid mold multiple times, this extends the life of the rigid mold
Soft mold must be rigid enough to survive imprint process and
transparent to allow crosslinking of photoresist
29. Januar 2015 Folie 10
Transmission Characteristics
• NXR-2010 crosslinks between 220nm and 300nm
• Multiple layers of Surlyn and Surlyn with PDMS backplane should allow
crosslinking of photoresist
29. Januar 2015 Folie 11
Embossing Results
• 1 layer of Surlyn – hard to handle (flimsy and curls on itself)
• 2 layers of Surlyn – easier to handle
• 3 layers of Surlyn – semi-rigid
• 4 layers – difficult to emboss (many corrugations)
• Surlyn from SONY (130-170 microns) – fairly rigid
PDMS backplane must be spin coated to get uniform thickness
Embossing is easier with Surlyn squares that fit within radius of wafer
although the entire pattern may not be transfered
29. Januar 2015 Folie 12
Imprinting Results
• Attempted to use several types of underlayers (TI-Prime/PMMA/NXR-3010)
• Used NXR-2010 undiluted and NXR-2010 + MMA(1:1)
Typically, ended with two results
• Photoresist ripped off, leaving few or no structures
• No crosslinking, leaving no structures (Bikini-Waxing)
29. Januar 2015 Folie 13
Imprinting Results: Ripping of Photoresist
29. Januar 2015 Folie 14
Imprinting Results: Bikini-Waxing
29. Januar 2015 Folie 15
Imprinting Results: Not a Total Loss
Some larger, partial structures
can be produced
29. Januar 2015 Folie 16
Imprinting Results
Conclusions:
1. Surlyn is too sticky
2. Thicker layers of Surlyn are not transparent
Recommendations:
1. Surlyn requires silanization or appropriate treatment
2. Create a rigid, negative mold using SiO2 wafer and NXR-2010 [1]
29. Januar 2015 Folie 17
Electrochemical Deposition of PANI on Au
29. Januar 2015 Folie 18
PANI Electrodeposition on Au
Basic Technique:
• Immerse electrodes in Aniline + H2SO4 solution
• Apply voltage bias across electrodes
• PANI will oxidize on cathode, grow, and “bridge” gap to the next electrode
Deposition Parameters:
• Voltage bias between electrodes (0.95V, 0.97, 1 V)
• Aniline Concentration (0.1 or 0.2 M Aniline)
• Deposition Times
Problems:
• Use of small drops to immerse electrodes can result in concentration
variation
• Little to no control of immersed electrode area
29. Januar 2015 Folie 19
PANI Electrodeposition on Au
Deposition Characteristics:
• Bridging times range from 45 minutes to
1.5 hours and more
• Conductance may grow steadily or rapidly in
orders of magnitude
• Bridging usually indicated by spikes in
current or relatively large current
• Current during deposition never
exceeds 10-4 A
29. Januar 2015 Folie 20
PANI Deposition on Au: Sample 5
Before Deposition
PANI Depositions
1. +0.95V, 1:10 hrs
2. +0.95V, 10 min
3. +0.95V, 5 min
Samples rinsed in Milli-Q water, blown dry, and
fresh Aniline solution added before each
deposit
After Deposition
After 3 depositions no
current between electrodes
when measured in air
29. Januar 2015 Folie 21
PANI Deposition on Au: Sample 5
No conduction because no bridging
29. Januar 2015 Folie 22
PANI Deposition on Au: Sample 5
Short period of low conductance to a jump in four orders of
magnitude in about 1 hr
29. Januar 2015 Folie 23
PANI Deposition on Au: Sample 5
Current on the order of 10-6 A, implies Aniline bridging between
electrodes
Non-linear characteristics
29. Januar 2015 Folie 24
PANI Deposition on Au: Sample 5
Some bridging between electrodes
Conductance ~ 10-6 A
29. Januar 2015 Folie 25
PANI Deposition on Au
Sample Average Deposition
Conductance (S)
Bridging Observed Conductance Near +1V
(S) measured in Air
3 10-9 No -
4 10-9 Yes 10-6
5 10-10 No
-
5b 10-4 Yes 10-6
6 10-9 Yes 10-7
7 10-7 Yes 10-6
8 10-9 No -
29. Januar 2015 Folie 26
PANI Deposition on Au: Voltage Dependence
0.1M Aniline, 0.95V
0.1M Aniline, 0.97V
0.1M Aniline, 1V
0.1M Aniline, 1V
29. Januar 2015 Folie 27
PANI Deposition on Au: Concentration Dependence
0.2M Aniline, 0.97V 0.2M Aniline, 0.95V
29. Januar 2015 Folie 28
Summary
Conclusions:
Surlyn soft molds need silanization
An SiO2 + NXR-2010 rigid mold may be an alternative to the soft mold
Deposition process not very predictable
Bridging will take 45 minutes or more
Use a funnel to control surface area and concentration
29. Januar 2015 Folie 29
Acknowledgments
Dr. Dirk Mayer
Dr. Andreas Offenhäusser
Nils Sanetra
Lynn Rathbun
Everyone from IBN-2
National Science Foundation
National Nanotechnology Infrastructure Network
Jennifer, Adam, and Kishore
Thanks For the Best Summer Ever!
29. Januar 2015 Folie 30
References
[1] Cross-linked Polymer Replica of a Nanoimprint Mold at 30 nm Half-pitch, Nano Lett., Vol. 5, No. 1,
2005

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Nano Elecrode Structures

  • 1. MitgliedderHelmholtz-Gemeinschaft 2009 iNNIN REU Electrochemical Deposition of Polyaniline on Nanoelectrode CrossBar Structures José Guevarra Department of Mechanical Engineering University of California, Santa Barbara PI: Dr Dirk Mayer Mentor: Nils Sanetra
  • 2. 29. Januar 2015 Folie 2 Outline • Motivation Molecular bioelectronics • The crossbar structure • Polyaniline (PANI) • Goals • Methods • Crossbar Structure Fabrication • Electrochemical deposition of PANI on Au • Summary and Outlook • Acknowledgments
  • 3. 29. Januar 2015 Folie 3 Molecular electronics What is molecular bioelectronics? • Miniaturization • Alternative to CMOS Bioelectronics • Biomolecule as active part • Totally new functions (e.g. sensor)
  • 4. 29. Januar 2015 Folie 4 The crossbar architecture What is a crossbar? • Two parallel planes of nanoscale wire arrays • Propterties of the crossbar determined by interjunction layer • Metal-Bridge-Metal (MBM) • For bioelectronics: Interjunctionlayer: SAM [Snider et al 2005]
  • 5. 29. Januar 2015 Folie 5 Polyaniline (PANI) • Well documented conducting polymer • Can be acid-doped to form conducting salt (emeraldine) • Can be electrochemically deposited • Cheap Can it be used to close the interjunction gap?
  • 6. 29. Januar 2015 Folie 6 Goals • Fabricate crossbar structures using a soft mold and lift-off process • Characterize pattern fidelity and compare to other methods • Electrochemically deposit a conducting polymer (Polyanaline) to bridge the junction gaps between crossbar junctions • Electronic characterization of polyaniline, electrodes, and junctions
  • 7. 29. Januar 2015 Folie 7 Methods
  • 8. 29. Januar 2015 Folie 8 Crossbar Structure Fabrication
  • 9. 29. Januar 2015 Folie 9 Fabrication Process (NanoImprint Lithography) CF4 Etch O2 Etch Gold Deposition Lift-Off Using a soft mold (Surlyn) allows one to imprint a pattern from a rigid mold multiple times, this extends the life of the rigid mold Soft mold must be rigid enough to survive imprint process and transparent to allow crosslinking of photoresist
  • 10. 29. Januar 2015 Folie 10 Transmission Characteristics • NXR-2010 crosslinks between 220nm and 300nm • Multiple layers of Surlyn and Surlyn with PDMS backplane should allow crosslinking of photoresist
  • 11. 29. Januar 2015 Folie 11 Embossing Results • 1 layer of Surlyn – hard to handle (flimsy and curls on itself) • 2 layers of Surlyn – easier to handle • 3 layers of Surlyn – semi-rigid • 4 layers – difficult to emboss (many corrugations) • Surlyn from SONY (130-170 microns) – fairly rigid PDMS backplane must be spin coated to get uniform thickness Embossing is easier with Surlyn squares that fit within radius of wafer although the entire pattern may not be transfered
  • 12. 29. Januar 2015 Folie 12 Imprinting Results • Attempted to use several types of underlayers (TI-Prime/PMMA/NXR-3010) • Used NXR-2010 undiluted and NXR-2010 + MMA(1:1) Typically, ended with two results • Photoresist ripped off, leaving few or no structures • No crosslinking, leaving no structures (Bikini-Waxing)
  • 13. 29. Januar 2015 Folie 13 Imprinting Results: Ripping of Photoresist
  • 14. 29. Januar 2015 Folie 14 Imprinting Results: Bikini-Waxing
  • 15. 29. Januar 2015 Folie 15 Imprinting Results: Not a Total Loss Some larger, partial structures can be produced
  • 16. 29. Januar 2015 Folie 16 Imprinting Results Conclusions: 1. Surlyn is too sticky 2. Thicker layers of Surlyn are not transparent Recommendations: 1. Surlyn requires silanization or appropriate treatment 2. Create a rigid, negative mold using SiO2 wafer and NXR-2010 [1]
  • 17. 29. Januar 2015 Folie 17 Electrochemical Deposition of PANI on Au
  • 18. 29. Januar 2015 Folie 18 PANI Electrodeposition on Au Basic Technique: • Immerse electrodes in Aniline + H2SO4 solution • Apply voltage bias across electrodes • PANI will oxidize on cathode, grow, and “bridge” gap to the next electrode Deposition Parameters: • Voltage bias between electrodes (0.95V, 0.97, 1 V) • Aniline Concentration (0.1 or 0.2 M Aniline) • Deposition Times Problems: • Use of small drops to immerse electrodes can result in concentration variation • Little to no control of immersed electrode area
  • 19. 29. Januar 2015 Folie 19 PANI Electrodeposition on Au Deposition Characteristics: • Bridging times range from 45 minutes to 1.5 hours and more • Conductance may grow steadily or rapidly in orders of magnitude • Bridging usually indicated by spikes in current or relatively large current • Current during deposition never exceeds 10-4 A
  • 20. 29. Januar 2015 Folie 20 PANI Deposition on Au: Sample 5 Before Deposition PANI Depositions 1. +0.95V, 1:10 hrs 2. +0.95V, 10 min 3. +0.95V, 5 min Samples rinsed in Milli-Q water, blown dry, and fresh Aniline solution added before each deposit After Deposition After 3 depositions no current between electrodes when measured in air
  • 21. 29. Januar 2015 Folie 21 PANI Deposition on Au: Sample 5 No conduction because no bridging
  • 22. 29. Januar 2015 Folie 22 PANI Deposition on Au: Sample 5 Short period of low conductance to a jump in four orders of magnitude in about 1 hr
  • 23. 29. Januar 2015 Folie 23 PANI Deposition on Au: Sample 5 Current on the order of 10-6 A, implies Aniline bridging between electrodes Non-linear characteristics
  • 24. 29. Januar 2015 Folie 24 PANI Deposition on Au: Sample 5 Some bridging between electrodes Conductance ~ 10-6 A
  • 25. 29. Januar 2015 Folie 25 PANI Deposition on Au Sample Average Deposition Conductance (S) Bridging Observed Conductance Near +1V (S) measured in Air 3 10-9 No - 4 10-9 Yes 10-6 5 10-10 No - 5b 10-4 Yes 10-6 6 10-9 Yes 10-7 7 10-7 Yes 10-6 8 10-9 No -
  • 26. 29. Januar 2015 Folie 26 PANI Deposition on Au: Voltage Dependence 0.1M Aniline, 0.95V 0.1M Aniline, 0.97V 0.1M Aniline, 1V 0.1M Aniline, 1V
  • 27. 29. Januar 2015 Folie 27 PANI Deposition on Au: Concentration Dependence 0.2M Aniline, 0.97V 0.2M Aniline, 0.95V
  • 28. 29. Januar 2015 Folie 28 Summary Conclusions: Surlyn soft molds need silanization An SiO2 + NXR-2010 rigid mold may be an alternative to the soft mold Deposition process not very predictable Bridging will take 45 minutes or more Use a funnel to control surface area and concentration
  • 29. 29. Januar 2015 Folie 29 Acknowledgments Dr. Dirk Mayer Dr. Andreas Offenhäusser Nils Sanetra Lynn Rathbun Everyone from IBN-2 National Science Foundation National Nanotechnology Infrastructure Network Jennifer, Adam, and Kishore Thanks For the Best Summer Ever!
  • 30. 29. Januar 2015 Folie 30 References [1] Cross-linked Polymer Replica of a Nanoimprint Mold at 30 nm Half-pitch, Nano Lett., Vol. 5, No. 1, 2005