Robert Cormia Michael Oye · Michael Oye UCSC El t i l E i i P f Robert Cormia Faculty Foothill College UCSC Electrical Engineering Professor Director, MACS Facility UCSC Associate

Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames

Michael OyeUCSC El t i l E i i P f

Robert CormiaFaculty Foothill College UCSC Electrical Engineering Professor

Director, MACS Facility UCSC Associate Co-Director, ASL

Faculty, Foothill CollegeNSF Principal Investigator

UCSC/NASA-ARC Advanced Studies Laboratories (ASL),NASA Ames Research Center,

Moffett Field, CA 94035ASL is a strategic alliance between NASA Ames Research Center and

the University of California Santa Cruz to foster collaboration between y f f z fAcademia, Government, and Industry


Outline:• Why Nanocarbon materials for Energy Storage? Ultracapacitors• Why Nanocarbon materials for Energy Storage? Ultracapacitors

• What is Nanocarbon?

• What is UCSC MACS Facility (and ASL)?What is UCSC MACS Facility (and ASL)?

• Synthesis

• Characterization

• NSF-funded training program for Synthesis & Characterization of Energy Storage materials for the Silicon Valley workforce


Nanocarbon Materials For Energy Storage:

WantHigh Energy Density andDensity and High Power Density;

Ultracapacitorsbring you closer

Source: http://www.websters-online-dictionary.org/images/wiki/wikipedia/commons/thumb/6/6b/Supercapacitors_chart.svg/350px-Supercapacitors_chart.svg.png


• Capacitor •Two plates that store electrical charge

Ult it• Ultracapacitor• Increase charge storage density through nanoporous material

• Activated carbon is most commonly usedct ated ca bo s ost co o y used•High surface-to-volume ratio•Relative low cost

Other types of carbon• Other types of carbon•Nanocarbons:

•Carbon Nanotubes•Graphenep•Nano-onions

•Others (Polymers, metal carbide MxCy, aerogels, and others)




• Synthesis



http://macs.advancedstudieslabs.orgCharacterization instruments available in UCSCCharacterization instruments available in UCSC MACS Facility at NASA Ames Research Center

in the Silicon Valley for Thin Film Users

SEM, with EDS(~1 nm resolution)

TEM, with EDS(~0.1 nm resolution)

XPS, QE/ICPE, metal & dielectric sputtering, and others tools.

•On site Technical Staff•On-site Technical Staff•Do-it-yourself, drop off samples, or mail in samples•On-line scheduling for reservations gand readily available instruments

See website forSee website for additional info

[email protected]://macs.advancedstudieslabs.org

y @

Hitachi H9500 Transmission Electron $129 $185TEM

Rates/hr for*: Non-profit Commercial

*Training rates l il bl Microscope

Hitachi S4800 Field Emission Scanning Electron Microscope

$83 $95SEM

are also available on the website

p

Hitachi TM1000 Tabletop Scanning Electron Microscope

$18 $30Tabletop SEM

Newport Oriel QE/IPCE Measuring Kit $18 $62

Perkin‐Elmer 5100 X‐ray Photoelectron $61 $90

QE/IPCE

XPS ray Photoelectron Spectroscopy (XPS) Unit

$61 $90

Technical Staff time $152 $200

XPS








Nanocarbon Synthesis

Spheres:GRAFEXTM

Rods:Carbon nanotubes using

Sheets:Plasma-enhanced

CVD of vertical

GRAFEXTM

Manufactured commercially by Clean Technology

International Corp. (CTIC); characterized in UCSC MACSChemical Vapor Deposition

(CVD) Furnace reactorsGraphene characterized in UCSC MACS

Facility at NASA Ameshttp://cticgroup.com/





• Synthesis



SEM (Hitachi S-4800): TEM:

100 nm 5 nm100 nm

Electron Microscope images taken by J. Varelas, on-site Technical Staff and Electron Microscopist

Graphite XPS SpectraSystem Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVMon Aug 09 14:42:00 2010

HOPG disk

Counts

420000

460000 Peak Label/ID Atomic % BE (eV)F 1s 0.3% 688.68O 1s 5.5% 532.48 C

1s

System Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVMon Aug 09 14:42:00 2010

HOPG disk

Counts

150000

170000 Peak Label/ID Atomic % BE (eV)F 1s 0.3% 688.68O 1s 5.5% 532.48C 1s 91 8% 283 88 C

-C

180000

220000

260000

300000

340000

380000 C 1s 91.8% 283.88Si 2p 2.5% 101.28

1s

70000

90000

110000

130000

C 1s 91.8% 283.88Si 2p 2.5% 101.28

C

Peak Label/ID BE (eV) FWHM (eV) Height Gauss %C-C 284.36 0.83 133928 70.0%C-C loss 285.50 2.62 10633.5 80.0%p-p* 290.15 3.00 2173.61 80.0%

Reduced Chi-Square: 9.61772

Binding Energy, (eV)02004006008001000

20000

60000

100000

140000

O A

uger

O K

LL-1

F K

LL-1

F 1s

O

Si 2

s

Si 2

pBinding Energy, (eV)

296 292 288 284 280

10000

30000

50000

C-C

loss

p-p*

S t N XY ASCIIHOPG di k S t N XY ASCIIHOPG di kSystem Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVMon Aug 09 14:42:00 2010

HOPG disk

Counts

20000

22000

24000 Peak Label/ID Atomic % BE (eV)F 1s 0.3% 688.68O 1s 5.5% 532.48C 1s 91.8% 283.88Si 2p 2.5% 101.28

C-O

, Si-O

System Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVMon Aug 09 14:42:00 2010

HOPG disk

Counts

2600

2700

2800 Peak Label/ID Atomic % BE (eV)F 1s 0.3% 688.68O 1s 5.5% 532.48C 1s 91.8% 283.88Si 2p 2.5% 101.28

C-F

x

12000

14000

16000

18000

C-O

Peak Label/ID BE (eV) FWHM (eV) Height Gauss %C-O, Si-O 532.14 1.59 12695.8 80.0%C-O 533.54 1.94 2625.09 80.0%


2000

2100

2200

2300

2400

2500 Peak Label/ID BE (eV) FWHM (eV) Height Gauss %C-Fx 689.11 2.14 841.4 80.0%


Binding Energy, (eV)542 538 534 530 526

8000

10000


1700

1800

1900

System Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVTue Apr 12 10:18:00 2011

nanocarbon grade 1

CountsSystem Name: XY ASCIIPass Energy: 100.00 eV

Nanocarbon grade 1

220000

260000

300000

340000Peak Label/ID Atomic % BE (eV)F 1s 0.1% 687.58O 1s 5.6% 532.48C 1s 94.1% 283.88Si 2s 0.2% 152.98

C 1

s

gyCharge Bias: 0.0 (0.0) eVTue Apr 12 10:18:00 2011Counts

80000

90000

100000

110000Peak Label/ID Atomic % BE (eV)F 1s 0.1% 687.58O 1s 5.6% 532.48C 1s 94.1% 283.88Si 2s 0.2% 152.98

C-C

P k L b l/ID BE ( V) FWHM ( V) H i ht G %

60000

100000

140000

180000

O A

uger

O K

LL-1

F 1s

O 1

s

2s 2p 30000

40000

50000

60000

70000

80000

C-C

, C-O

C, C

=O

*

Peak Label/ID BE (eV) FWHM (eV) Height Gauss %C-C 284.31 1.27 92105.4 75.0%C-C, C-O 285.94 1.50 10568.7 85.0%C-C, C=O 287.69 2.05 4615.93 85.0%p-p* 290.11 2.51 2951.43 85.0%



20000 Si

Si


10000

20000

C

C-C

p-p*

S t N XY ASCIIN b d 2System Name: XY ASCIINanocarbon grade 2

System Name: XY ASCIIPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVTue Apr 12 10:18:00 2011

Nanocarbon grade 2

Counts

260000

300000

Peak Label/ID Atomic % BE (eV)O 1s 0.4% 532.48C 1s 99.3% 284.98Si 2p 0.2% 102.38

C 1

s

yPass Energy: 100.00 eVCharge Bias: 0.0 (0.0) eVTue Apr 12 10:18:00 2011

g

Counts

140000

160000

180000Peak Label/ID Atomic % BE (eV)O 1s 0.4% 532.48C 1s 99.3% 284.98Si 2p 0.2% 102.38

C-C

Peak Label/ID BE (eV) FWHM (eV) Height Gauss %

100000

140000

180000

220000

260000

60000

80000

100000

120000

140000

C-O

=O

Peak Label/ID BE (eV) FWHM (eV) Height Gauss %C-C 284.41 0.94 150941 75.0%C-C, C-O 285.82 1.50 13024.4 85.0%C-C, C=O 288.00 2.00 2745.88 85.0%p-p* 290.74 2.56 3693.68 85.0%



20000

60000

100000

O K

LL-1

O 1

s

Si 2

s

Si 2

p


20000

40000

C-C

,

C-C

, C=

p-p*

Sample 21 (Functionalized) Raman Peak Analysisy





• Synthesis



Overview:• Incumbent Training• Incumbent Training

• Hitachi S-4800 SEM

• Hitachi H-9500 TEM

• Thin Film Deposition

• Carbon Deposition



SEM: S-4800:Sample preparation

TEM: H-9500:Sample preparationSample preparation

Instrument loadingImage acquisitionEDX/EDS analysis

Sample preparationInstrument loadingImage acquisitionEDX/EDS analysisy y

Thin Film Deposition:V ti

Nanocarbon Deposition:G h dli f t•Vacuum operation

•Target selection / parameters•Operating feedback•Step height analysis

•Gas handling safety•Gas monitoring•Plasma operation•Growth parameters•Step height analysis

•EDX thin film analysis•Growth parameters•Characterization

Multiple stages of a launching careerlaunching career

cation

Edu

Vision: Individually Customizable Student Training and Development ProgramStudent Training and Development Program

Pre-college

A.A./B.A.

B.A./B.S. Doctorate

Post-Doctoral

M.A./M.S.

More on-ramps & Examples: Internships Militarypoff-ramps;

Examples: Internships, Military careers, Jobs, Family, etc.


Contact Info:Robert Cormia, [email protected], @Michael Oye, [email protected]://macs.advancedstudieslabs.org

Acknowledgements:• M. Meyyappan, NASA, Chief Scientist for Exploration Technology and Former Director, NASA Ames Center for Nanotechnology• B Chen Zuki Tanaka Raman Spectroscopy• B. Chen, Zuki Tanaka, Raman Spectroscopy •W. Vercoutere, B. Le Boeuf, P. Minogue, J. Varelas, N. Kobayashi, T. Siegel, G. Ringold, S. Zornetzer, ASL Management team•P. Murray, Foothill College Dean•J Gacusan W Page D Mo E Sandoz Rosado D O’Brien S Takahashi Nanocarbon growths•J. Gacusan, W. Page, D. Mo, E. Sandoz-Rosado, D. O Brien, S. Takahashi, Nanocarbon growths•Danny Cross, Tom Strickland, Steve Wallace, Clean Technology International Corp. (CTIC)

Documents

Robert Cormia Michael Oye · Michael Oye UCSC El t i l E i i P f Robert Cormia Faculty Foothill College UCSC Electrical Engineering Professor Director, MACS Facility UCSC Associate