robert cormia michael oye · michael oye ucsc el t i l e i i p f robert cormia faculty foothill...
TRANSCRIPT
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
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
• 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 and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
Outline:• Why Nanocarbon materials for Energy Storage? Ultracapacitors• Why Nanocarbon materials for Energy Storage? Ultracapacitors
• What is Nanocarbon?
• Synthesis
• Characterization
• NSF-funded training program for Synthesis & Characterization of Energy Storage materials for the Silicon Valley workforce
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
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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)?
• Characterization
• NSF-funded training program for Synthesis & Characterization of Energy Storage materials for the Silicon Valley workforce
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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 and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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
• NSF-funded training program for Synthesis & Characterization of Energy Storage materials for the Silicon Valley workforce
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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%
Reduced Chi-Square: 3.16078
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%
Reduced Chi-Square: 2.87188
Binding Energy, (eV)542 538 534 530 526
8000
10000
Binding Energy, (eV)698 694 690 686 682
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%
Reduced Chi-Square: 4.67448
Binding Energy, (eV)02004006008001000
20000 Si
Si
Binding Energy, (eV)296 292 288 284 2800
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%
Reduced Chi-Square: 13.4131
Binding Energy, (eV)02004006008001000
20000
60000
100000
O K
LL-1
O 1
s
Si 2
s
Si 2
p
Binding Energy, (eV)296 292 288 284 2800
20000
40000
C-C
,
C-C
, C=
p-p*
Sample 21 (Functionalized) Raman Peak Analysisy
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
Overview:• Incumbent Training• Incumbent Training
• Hitachi S-4800 SEM
• Hitachi H-9500 TEM
• Thin Film Deposition
• Carbon Deposition
• NSF-funded training program for Synthesis & Characterization of Energy Storage materials for the Silicon Valley workforce
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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.
Synthesis and Characterization of Nanocarbonusing the UCSC MACS Facility at NASA Ames
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)