1. Project #4 Manufacture and Characterization of Carbon Nanotube Microcable Sponsored By The National Science Foundation Grant ID No.: DUE-0756921 Timothy Ochmann(Pre-Junior ChE) & Nicholas Kienzle(Pre-Junior ChE) Faculty Mentors: Dr. Vesselin Shanov & Dr. Noe Alvarez SEEMBE College of Engineering and Applied Science; University of Cincinnati; Cincinnati, Ohio 04.04.13 3:30 P.M. 1

2. Outline Background Goals Process Results 2

3. Discovery Russia 1952 1 Japan 1991 2 3 1..LV Radushkevich and VM Lukyanovich. "The structure of the carbon produced by the thermal decomposition of carbon monoxide on iron contact." ЖФХ, 26, 88 (1952)) 2.Iijima, S., “Helical microtubules of graphitic carbon”,. Nature 354, 56 - 58 (1991)

4. Background Cont. 4 3. http://people.bath.ac.uk/tl258/Types.html Figure : Singlewall Carbon Nanotube vs. Multiwall Carbon Nanotube 3

5. Background Cont. As Spun CNT Thread – Conductivity of 3.8 * 10 4 S/m Future use in Power Distribution High Cycle Fatigue, Corrosion Resistant 5

6. Background – Band Gap Gap between Conduction Band and Valence band Attempting to “close” the gap using various chemicals Determines Electrical Properties of material Exohedral Doping to solve problem 6 Coating CNT thread Metals 2.http://www2.warwick.ac.uk/fac/sci/phttp://www2.warwick.ac.uk/fac/ sci/physics/current/postgraduate/regs/mpags/ex5/bandstructure/hysi cs/current/postgraduate/regs/mpags/ex5/bandstructure/

7. Project Goals Increase Conductivity of CNT thread Coat CNT thread for insulation Create demonstration for enhanced CNT thread properties as an electrical wire Fully characterize CNT thread (mech. strength, electrical, Raman spectroscopy) NOTE: work is towards continuing progress in electrical and strength improvements for use as a super fiber in future 7

8. Chemical Vapor Deposition Figure 3: Schematic of CVD system 4 8 4. Ge Li, Supriya Chakrabarti, Mark Schulz, Vesselin Shanov, Carbon, Volume 48, Issue 7, June 2010, Pages 2111-2115, ISSN 0008-6223, 10.1016/j.carbon.2010.01.054. Note: Using Si substrate C 2 H 4 (g) in Ar(g) carrier gas

9. Dry Spinning CNT Array into CNT Thread 9

10. Dry Spinning at UC Nanoworld 10

11. Scanning Electron Microscope (SEM)- As spun CNT Thread 11 Figure 8: SEM image of CNT thread as spun. Image taken 08.30.12.

12. Doping Method Liquid phase doping Stand holds bobbin CNT thread is drawn from solution for drying 12

13. Post Treatment Agents Dopants Nitric Acid Potassium Tetrachloroaurate (III) Solvents Acetone DMSO N-methyl-pyrrolidone 13 Exohedral Doping

14. SEM Image – Acetone Densified CNT Thread 14 Figure 9: SEM image of CNT thread with post processing. Image taken 08.30.12.

15. SEM Image – Au/HNO 3 Doped CNT Thread 15 Figure 10: SEM image of CNT thread after Au/Nitric Acid Doping 5 5. Noe Alvarez, Ruff, Haase, Malik, Kienzle, Mast, Schulz, Shanov, Recent Advances in Circuits, Communications and Signal Processing

16. Polymer Coating for Wire Insulation 16 Collecting bobbin Heater Polymer Bath Hydrogenated Nitrile Butadiene Rubber Dissolved in Butyrate Thinner from Randolph Aircraft Finisher with cross linking agent LUPEROX ® 101

17. SEM Image – Nitrile Polymer Coated CNT Thread 17 5. Noe Alvarez, Ruff, Haase, Malik, Kienzle, Mast, Schulz, Shanov, Recent Advances in Circuits, Communications and Signal Processing Figure 11: SEM image of CNT thread after Hydrogenated Nitrile Butadiene Rubber Coating 5

18. Characterization – 4 Point Probe Resistance Test Silver paint was used to attach the CNT thread to the pins. 18 I = current supplied V = Voltage Figure 11: 5 pin connector used as a template for 4 point probe resistance test (test length of 4.2 mm with silver paste connections

19. Tensile Strength Improvement 19 Ultimate Tensile Strength Improves Elastic Modulus Improves (Stress/Strain) Toughness improves CNT Thread Name Average Ultimate Stress (MPa) Average Moduli (GPa) Average Toughness (MPa) AP71 Reference 115.564.70932.3416 AP71 Au Doped 338.5523.8084.2526

20. Raman Spectroscopy 20 D Peak G Peak G’ Peak D Peak – presence of sp 2 hybridized G Peak – Graphitic peak G’ Peak – second vibrational mode of CNT D:G Ratio – measure of amorphous carbon on surface as well as other defects

21. Raman Spectroscopy - Coated Spectrum for HNBR 21 6. K.D.O. Jackson, M.J.R. Loadman, C.H. Jones, G. Ellis, Fourier transform raman spectroscopy of elastomers: An overview, Spectrochimica Acta Part A: Molecular Spectroscopy, Volume 46, Issue 2, 1990, Pages 217-226, ISSN 0584-8539, 10.1016/0584-8539(90)80091-C. 1 2 21 Spectrum for HNBR Coated

22. Application - Microcable 22

23. Conclusion Properties Au Doped CNT Thread Literature 6 Copper Conductivity (S/m) 1.37*10 5 6.67*10 6 5.96*10 7 Density (g/cm^3) ~1.0 8.96 23 6. Yao Zhao,Jinquan Wei1, Robert Vajtai, Pulickel M. Ajayan, and Enrique V. Barrera “Iodine doped carbon nanotube cables exceeding specific electrical conductivity of metals”, Nature, September 2011

24. Acknowledgements Dr. Vesselin Shanov and Dr. Mark Schulz (lab directors of Nanoworld Labs) Dr. Noe Alvarez and Dr. Weifeng Li (post doctorates) Mark Haase, Rachit Malik, Joe Sullivan, Adam Hehr, Brad Ruff (graduate students) Doug Hurd (machine shop director) National Science Foundation for funding our work General Nano LLC (facilities for catalyst preparation) 24