Process steps for Field Emitter devices built on Silicon wafers And 3D Photovoltaics on Silicon wafers

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1 Process steps for Field Emitter devices built on Silicon wafers And 3D Photovoltaics on Silicon wafers David W. Stollberg, Ph.D., P.E. Research Engineer and Adjunct Faculty GTRI_B-1

2 Field Emitters GTRI_B-2

3 Doped Si GTRI_B-3

4 Deposit SiO2 (~10mm) Variable for Height SiO 2 Doped Si GTRI_B-4

5 Deposit gate (poly Si or Cr, ~200nm) poly-si SiO 2 Doped Si GTRI_B-5

6 Doped SiO 2 Si poly-si plan view Spincoat Photoresist poly-si SiO 2 Doped Si elevation view GTRI_B-6

7 Doped SiO 2 Si Pattern Develop poly-si plan view Resist poly-si SiO 2 Doped Si elevation view GTRI_B-7

8 Etch gate and insulator isotropically Doped SiO 2 Si poly-si poly-si SiO 2 plan view Resist Doped Si elevation view GTRI_B-8

9 Deposit catalyst metal Fe shown Ni possible with barrier layers Doped SiO 2 Si poly-si poly-si SiO 2 plan view Fe catalyst Resist Doped Si elevation view GTRI_B-9

10 Doped SiO 2 Si poly-si Lift off & Dice plan view poly-si SiO 2 Doped Si elevation view GTRI_B-10

11 Doped SiO 2 Si poly-si Grow CNTs plan view poly-si SiO 2 Doped Si elevation view GTRI_B-11

12 Connect and HPEPL Langmuir Probe Doped SiO 2 Si poly-si e- plan view e- e- poly-si SiO 2 V Doped Si Measure I, V elevation view GTRI_B-12

13 GTRI_B-13

14 CNT growth parameter for CNTs 2µm CVD growth: N 2 and NH 3 flowed at 100sccm and 160scmm Temperature ramp of 300 C/min until 650 C (top and bottom heat) Annealed at 650 C for 2min Plasma Ignited: 80W, 15kHz, 800V Pressure controller activated: P chamber = 6mbar Annealed under NH 3 plasma for 3 min while T raised to 750 C at rate of 200 C/min C2H2 (40sccm) introduced at end of plasma anneal Growth time = 6min Plasma extinguished, cooled under N 2 flow until T <400 C. Opened to atmosphere GTRI_B-14

15 Influence of Temperature on CNT growth Below 725 C Catalyst does not sufficiently create synthesis islands. Short, fat Carbon Fiber like CNTs result Around 725 C islands initiate growth, but rate of growth is limited 750 C - growth rate of ~0.3µm/min 775 C some smaller islands, higher growth rate of smaller diameter CNTs 800 C increased Ni diffusion into Si, few catalyst island remain on surface, sparse CNT growth, much lower diameter. Rate is similar to range with larger variance 650 C 675 C 700 C 725 C GTRI_B C 775 C 800 C

16 Ion Electric Propulsion G. Pirio, et al, Nanotechnology, vol. 13, pp. 1-4, Electron-induced Surface Plasmon Resonance (Chem-Bio Sensor) MRE Antibodies Y Y Y Y Y Gold Foil Gate CNTs TiW/Mo/TiW electrode GTRI_B-16

17 84 Emitter Capacity 2.1 A at 25 ma/cm2 Busek BHT-200 Modified for use with CNT Emitters GTRI_B-17

18 Thrust! GTRI_B-18

19 3D Solar Cells GTRI_B-19

20 Multiple bounce light trapping Light Trapping= more absorbance Thinner layers = less recombination orthogonalize absorption and carrier extraction Solves thick-thin conundrum GTRI_B-20

21 CNT-Based Approach PR spun on PR Si GTRI_B-21

22 CNT-Based Approach UV PR spun on Mask and expose to UV PR Mask Si GTRI_B-22

23 CNT-Based Approach PR spun on Mask and expose to UV Develop PR PR PR Si GTRI_B-23

24 CNT-Based Approach PR spun on Mask and expose to UV Develop PR Fe deposited metal PR PR Si GTRI_B-24

25 CNT-Based Approach Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst metal metal Si GTRI_B-25

26 CNT-Based Approach CNT Tower metal CNT Tower metal Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) Si GTRI_B-26

27 CNT-Based Approach Pattern generated on Si substrate via photolithography CNT Tower metal p-type Si CNT Tower metal Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) p-type material (CdTe) applied via Molecular Beam Epitaxy (MBE) GTRI_B-27

28 CNT-Based Approach CNT Tower metal n-type p-type Si CNT Tower metal Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) p-type material (CdTe) applied via Molecular Beam Epitaxy (MBE) n-type material (CdS) applied via MBE or CBD GTRI_B-28

29 CNT-Based Approach CNT Tower metal TCO n-type p-type Si CNT Tower metal Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) p-type material (CdTe) applied via Molecular Beam Epitaxy (MBE) n-type material (CdS) applied via MBE or CBD Transparent Conductive Oxide applied via ion assisted deposition (IAD) GTRI_B-29

30 CNT-Based Approach CNT Tower metal TCO n-type p-type Si CNT Tower metal h u Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) p-type material (CdTe) applied via Molecular Beam Epitaxy (MBE) n-type material (CdS) applied via MBE Transparent Conductive Oxide applied via ion assisted deposition (IAD) V GTRI_B-30

31 CNT-Based Approach h u Pattern generated on Si substrate via photolithography Metal catalyst (Fe) applied Lift-off photoresist to leave only patterned catalyst atop interconnect layer CNT towers are formed in Chemical Vapor Deposition (CVD) furnace (~720 C; 20 min.) p-type material (CdTe) applied via Molecular Beam Epitaxy (MBE) n-type material (CdS) applied via MBE Transparent Conductive Oxide applied via ion assisted deposition (IAD) GTRI_B-31

32 Molecular Beam Epitaxy for CdTe and CdS deposition (p/n junction) CdTe CNTs CNTs Si substrate GTRI_B-32

33 GTRI_B-33

34 GTRI_B-34

35 Reflectance, R (%) Light Reflection Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample Wavelength, (nm) GTRI_B-35

36 Extra Slides on CNT Batteries GTRI_B-36

37 Silicon Battery Si-coated Carbon Nanotubes for Li - ion battery anodes (with Yushin in MSE) Silicon has an order of magnitude greater capacity compared to graphite anodes But Silicon has very poor cyclability (pulverizes with Lithium insertion) Solution = Reinforce Silicon (with Carbon Nanotubes) 1 5 kc 1 Li e Si LixSi x 22 ka x 5 22 GTRI_B-37

38 Vertically aligned carbon nanotubes Act as rebar to strengthen internal structure of Si-battery Pictures of Si-coated Carbon Nanotubes Demonstrates conformal coatings are possible GTRI_B-38

39 Dealloying Capacity (mah/g) Coulombic Efficiency (%) Charge/Discharge Results C-Si-VACNTs Theoretical capacity of graphite Cycle Number Stable performance and reversible dealloying capacity in excess of 2000 mah/g (over 5x more than graphite) has been demonstrated. VACNTs provide structural support for Si as well as dramatically improved electrical conductivity therefore higher power Sicontaining electrodes are possible. GTRI_B-39

40 : Sensors Cultures Scaffolds 100 mm Heat Sink Batteries 20 mm Fuel Cells Logic circuits Hydrogen storage Waveguide/Filter Many, MANY more... 1 mm GTRI_B-40

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