chem_iitd_feb2015_thin film growth with ced
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Thin Film Coating Using
Cathodic Arc
Irfan Irfan Alameda Applied Sciences Corp. San Leandro (the SF Bay Area), California
`
This research is supported at AASC by DOE SBIR Grants DOE Grants: #DE-SC0011371, DE-SC0011294,
DE-SC0007678, DE-SC0004994 and DE-SC0009581
At Department of Chemistry IIT-Delhi on 10 February 2015
Small R&D firm, started in
1994 by Dr. Mahadevan
Krishnan.
Since inception main focus
has been the application of
Pulsed Plasma Technology.
Funded substantially by
different government
contracts.
Alameda Applied Sciences Corporation:
Limited success in past
commercialization
attempts.
Currently more focused on
SRF coatings and fast gas
valves for LPA.
Alameda Applied Sciences Corp. Contd.:
Cathodic Arc Coating (Ion Energy):
Comparison of Stress build-up in low energy deposition, energetic condensation, and energetic condensation plus high voltage bias
[*] M. M. Bilek, R N. Tarrant, D. R. McKenzie, S H. N. Lim, and D G. McCulloch “Control of Stress and Microstructure in Cathodic Arc Deposited Films” IEEE TRANSACTIONS ON PLASMA SCIENCE, VOL. 31, NO. 5, OCTOBER 2003
(A. Bendavid, CSIRO)
(M.M. Bilek)
* A. BENDAVID, P. J. MARTIN, R. P. NETTERFIELD, G. J.
SLOGGETT, T. J. KINDER, C., ANDRIKIDIS, JOURNAL OF
MATERIALS SCIENCE LETTERS 12 (1993) 322-323
Ion energy, eV
f(e)
Nb
Energetic Condensation (Crystal Growth):
In Energetic Condensation, the ions deposit energy in a sub-surface layer (≈3-5 atomic
layers deep for ~100eV Nb ions), shaking up the lattice, causing adatom mobility and
promoting epitaxial crystal growth
Energetic Condensation, when combined with substrate heating, promotes lower-defect
crystal growth
J.A. Thornton, "Influence of substrate temperature and deposition rate on the structure of thick sputtered Cu coatings”, J. Vac. Sci.
Technol. Vol. 12, 4 Jul/Aug 1975
Andre Anders, A structure zone diagram including plasma-based deposition and ion etching, Thin Solid Films 518 (2010) 4087–4090
~30-100 V applied between a desired cathode and an anode mesh.
A triggering event at one side initiates one pulse of coating.
Averaged over many pulses it creates a uniform ~1 monolayer/pulse coating.
Coaxial Energetic Deposition:
Coaxial Energetic Deposition (CEDTM)
SRF Coating Requirements:
Test Why
Film ADHESION with frequent cooling
and heating: Thermal Shocks
For operation at 2-4 oK
Film ADHESION with >500 psi water
rinse: Mechanical Shocks
To remove particulates and secondary
ion emission sites
Film ADHESION with: Mechanical
Flex
For connecting RF cavities/cells
(stainless steel bellows)
High Crystalline growth: High RRR For acceleration gradient in >1010
eV/m (no quenching) => Low
resistance (BCS limit and low defects)
Compatibility with Complex
Geometries
For coating real accelerator hardware,
RF cells, Power Couplers
In Liquid nitrogen bath multiple times.
Tested at AASC
Thermal Shock:
In Liquid nitrogen bath multiple times.
Tested at Brookhaven National Lab by J C Brutus, B. Ping, and Y. Huang.
Thermal Shock on Bellows:
CERN Resonator Plate-1:
The film came off at
~8 bars (~60psi)
High pressure water rinse (HPWR) on ~3 mm thick12 mm x 50 mm bars.
All survived well beyond 500 psi.
Tested at Fermi Lab by Curtis Crawford
Mechanical Shock:
CERN Resonator Plate-II:
5 min. in a 20g/l sulfamic acid -> 20 min. rinse in distilled water -> in IPA bath till mounting.
3.4 micron film at center and ~2 around edges.
Survived ~80 psi at CERN, tested by Sarah Aull.
The Nb film survived repeated cycles of HPWR at up to (80Bar) 500psi.
Tested at Los Alamos N Lab by T. Tajima
Nb Coated Cu 1.3 GHz Cell:
KEK-06 Cu cavity before Nb coating KEK-06 Cu cavity after Nb coating
Mechanical Flex on Bellows:
Starts in Expanded position 3.5”
Compressed to 2.6” in 1 sec,
stays 0.5 sec
Back to expanded position in 1
sec, stays 0.5 sec
24,000 times (~20 Hrs)
Rinsed, filtered and analyzed for
particles that may come off
during the mechanical flex test
Tested at BNL by Bin Ping et al
High RRR films:
HPWR 500 psi at FNAL, RRR≈52 in our Cu films
Temple Univ. measured AASC Cu on SS strips RRR~42 – 64
XFEL Germany requirements >30
Stainless steel tube coated with a ~28µm
Cu film using the AASC CED process
Copper surface after 86Bar HPWR test
(courtesy of Curtis Crawford/FNAL)
High RRR on coupons motivates coating accelerator structures
RRR-585 measured on 5µm
film on MgO
RRR-330 measured on a-
sapphire
M Krishnan, E Valderrama, B Bures, K Wilson-Elliott, X Zhao, L Phillips, A-M Valente-Feliciano, J Spradlin, C
Reece and K Seo, “Very high residual-resistivity ratios of heteroepitaxial superconducting niobium films on MgO
substrates,” Superconductor Science and Technology , vol. 24, p. 115002, November 2011
M. Krishnan, E. Valderrama, C. James, X. Zhao, J. Spradlin, A-M Valente Feliciano, L. Phillips, and C. E. Reece,
K. Seo, Z. H. Sung, “Energetic condensation growth of Nb thin films”, PHYSICAL REVIEW SPECIAL TOPICS -
ACCELERATORS AND BEAMS 15, 032001 (2012).
110 & 200 200 110
Polycrystalline
Monocrystal
with two
orientations
Monocrystal
with 100
orientation
RRR=7, 150/150 RRR=181, 500/500 RRR=316, 700/700
Change in crystal
orientation from 110 to 200
at higher temperature
RR
R
RR
R
Compatibility with Complex Geometries:
Coating inner surface of bellows.
Coating outer surface of tubes.
Coating inner surface of long tubes.
HPWR 500 psi at FNAL all survived except the
tube coated outside.
RF test of Nb Film:
Nb coating on 2” Cu single crystal.
RF measurement by Paul Welander at SLAC-Stanford.
Current State of the Art Bulk Nb:
N doped bulk Nb cavities from FNAL.
AASC Nb coating on KEK06, RF measurements by T. Tajima at LANL.
1.E+05
1.E+06
1.E+07
1.E+08
1.E+09
0 2 4 6 8 10
Q0
Eacc(MV/m)
4K
<2K
Thank You AASC
Mahadevan Krishnan,
Steven Chapman,
Katherine Velas Los Alamos N. Lab
Tsuyoshi Tajima.. CERN
Sarah Aull..
Fermi Lab
Curtis Crawford,
Lance Cooley..
Brookhaven N. Lab
Sergey, Bin Ping..
Jefferson Lab
Rong Li, C. Reece…
Argonne N. Lab
Thomas Prolier..
SLAC (Stanford)
Paul Welander..
SLAC (Stanford)
Xiaoxing Xi..
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