a15 superconductors - · pdf fileessence of the previous slides. testardi, 1975 literature:...
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A15 Superconductors:Alternative to Nb for RF CavitiesS.M. Deambrosis*^, G. Keppel*, V. Palmieri*^, V. Rampazzo*^,
C. Roncolato*, R.G. Sharma°, F. Stivanello*
Padova University, Material Science Dept
* INFN - Legnaro National Labs^ Padua University, Science faculty, Material Science Dept
° Nuclear Science Centre, New Delhi
Outline
• Theory: Surface Resistance
– Mo-Re system: Deposition Technique and Results
– V3Si: Thermal Diffusion in Reactive SiH4 Atmosphere
– Nb3Sn: Liquid solute diffusion tecnique
– 6 GHz cavities: RF Measurements
• Conclusions and future plan
Zn = 1 − iσnδ
= 1 − iρnδ
σ1-iσ2 in place of σn
Surface Impedance and Surface Resistance
For a normal metal in the normal regime:σn = 1 / ρn = dc conductivity at T
δ = skin depth
As derived by Nam, for T < Tc / 2, Rs can be approximated by:
2
1
3
2
12n
ns
n
RR σ
σ
σσ
⎛ ⎞⎜ ⎟⎝ ⎠
=
Extension to Superconductors:
( ) ( ) ( )1 2
n
f E f E g E dEσσ
ωω
∞+
∆
= + +⎡ ⎤⎣ ⎦∫ hh
( ) ( ),
2 1 1 2n
f E g E dEω
σσ
ωω
∆−
∆ − − ∆
= − +⎡ ⎤⎣ ⎦∫h
hh
In the framework of the BCS theory, for ω < 2 ∆, the complex conductivity of a superconductor is:
Mattis and Bardeen Integrals
The two integrals σ1/σn and σ2/σn are easily numerically calculated.
In the normal skin effect regime, for ħω << 2 ∆
( )2/
/1
2
ln1
B
B
B
K T
K T
n
K T
eeσ
ωσ−
−∆
∆
∆⎡ ⎤⎢ ⎥ ∆⎢ ⎥=⎢ ⎥+⎢ ⎥⎣ ⎦
h
2 tanh2n BK T
σσ
πω∆ ∆
=
( )( )TOeARR TKn
n
nBCS
B ,,12
123
ωρσσ
πω
∆+=⎟⎠⎞
⎜⎝⎛
∆≅
∆−h
RBCS
Then, if T < Tc / 2
Empirically, Rres is found to be dependent on ρn too.
For low rf losses,
a high TC value is not sufficient
A metallic behaviourin the normal state is mandatory
Essence of the previous slides
Testardi, 1975
Literature: Mo-Re system
Mo38Re62
Mo40Re60Mo65Re35
Literature: Mo-Re system
A – Sputtering v ~ 500 Å/min, deposition T = 1000 °C, B – Sputtering v ~ 1000 Å/mindeposition T = 1200 °C, C – Mo-Re bulk samples
Gavaler et al.
Mo-Re system: deposition tecnique
Magnetron Sputtering at high T
3 Target Compositions
Mo75Re25
Mo38Re62
Mo60Re40
26 SPUTTERING RUNS
11 samples SETS
More than 60 samples
Annealing treatment
Mo75Re25
Mo75Re25: XRD Spectra
44,49 64 ,49 84 ,49 104 ,49 124 ,49 144 ,49
0
20
40
60
80
100
Rel
ativ
e In
tens
ity
An g o lo 2 ϑ (g ra d i)
(110)
(200)
(211)
(220)(310)
(222)
(321)
Film XRD Spectrum
Deposition T = 633°C, Annealing t = 15 minutes
Target XRD Spectrum
11,0 11,2 11,4 11,6 11,8 12,0 12,2-0,002
0,000
0,002
0,004
0,006
0,008
0,010
0,012
0,014
0,016
R (Ω
)
T (K)
Tc = 11.398K∆Tc = 0.009KRRR = 1.57
Mo75Re25: A Superconductive Transition Curve
Deposition T = 633°C Annealing t = 15 min
0 5 10 15 20 25 3011,2
11,3
11,4
11,5
11,6
11,7
11,8
11,9T c (
K)
Annealing time (minutes)
Deposition T = 750°C Deposition T = 800°C
Mo75Re25: Tc vs Annealing Time
0 Gauss
Mo75Re25: R vs T at Increasing H
4,5 5,0 5,5 6,0 6,5 7,0 7,5 8,0 8,5 9,0 9,5 10,0 10,5 11,0 11,5-0,002
0,000
0,002
0,004
0,006
0,008
0,010
0,012
0,014
0,016R
(Ω)
T (K)
Deposition T = 633°C, Annealing t = 15 minutes
40 000 Gauss
8 9 10 11 12-0,0372
-0,0370
-0,0368
-0,0366
-0,0364
-0,0362
-0,0360
-0,0358
M' (
emu)
T (K)
Mo75Re25, Cu: Deposition T = 680°C, no annealing
A Mo75Re25 Film Deposited on Cu
Tc = 11.18K∆Tc = 0.08K
A Mo75Re25 Film Deposited on Nb
8 9 10 11 12
-0,028
-0,026
-0,024
-0,022
-0,020
-0,018
-0,016
-0,014M
' (em
u)
T (K)
Mo75Re25, Nb: Deposition T = 725°C, Annealing t = 15 min
Tc = 11.03K∆Tc = 0.08K
Nb
Mo75Re25
11,8 11,9 12,0 12,1 12,2 12,3 12,4
0,000
0,005
0,010
0,015
0,020
R (Ω
)
T (K)
Mo60Re40: A Superconductive Transition Curve
Deposition T = 750°C Annealing t = 60 min
Tc = 12.00K∆Tc = 0.041KRRR = 1.88
0,0 0,5 1,0 1,5 2,0
0,05
0,06
0,07
0,08
0,09∆
T c (K
)
Annealing time (h)
Deposition T = 800°C Deposition T = 850°C
Mo60Re40: ∆Tc vs Annealing Time
Lines of equal RBCS. At T = 4.2 K, f = 500 MHz, s = 4
RBCS depends on ∆ and ρn
Nomogram
Mo60Re40 (Tc = 12.13, RRR =1.3, ρn ~ 30µΩcm ),
Mo75Re25 (Tc = 11.82, RRR =1.71, ρn ~ 10µΩcm).
9.0 9.5 10.0 10.5 11.0 11.5
0.00
0.02
0.04
0.06
0.08
0.10
0.12
0.14
0.16
T (K)
R (Ω)
Mo38Re62: A Superconductive Transition Curve
Deposition T = 750°C, Annealing t = 60 minutes
Tc = 9.47K∆Tc = 0.029KRRR = 1.11
• Annealing treatments give surprising results: >Tc,<∆Tc
• Tc is higher than 12K (Mo60Re40)
• Long range order is very important so ∆Tc becomes one of the most meaningful parameters. A sharpsuperconducting transition corresponds to a high ξ0.
Essence of the previous slides
• We deposited more than 100 films
• RBCS is around 16 nΩ (Mo75Re25, Mo60Re40)
V3Si: RRR vs Silicon content
Preliminary results on cosputtering of V3Si films by the facing-target magnetron technique
Y. Zhang, V. Palmieri, R. Preciso, W. Venturini, Legnaro National Laboratory, ITALY
Schematic diagram of the facing-target magnetron.
V target Si target
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
13.5 14.0 14.5 15.0 15.5 16.0 16.5
sample5-9RR
K
Superconducting transition of a V3Si sample
RR
R
Thermal diffusion of V3Si filmsY. Zhang, V. Palmieri, W. Venturini, F. Stivanello, R. Preciso, Legnaro National Laboratory, ITALY
40h20h900ºC300W1.2·10-4mbar
Anneal in vacuum
Diffuse in silane
TemperatureHeat powerSilane pressureDiffusion
Parameters:
There is room to improve the film quality by higher thermal diffusion temperature or by longer annealing time in vacuum.
2.5
3.0
3.5
4.0
4.5
14.5 15.0 15.5 16.0 16.5 17.0
Bulk Vanadium, sample No.13-2V
K
AC inductive measurement:Tc ~ 16.0K ∆Tc < 0.4K
6.0
9.0
12.0
15.0
18.0
10.0 15.0 20.0 25.0 30.0Silicon content ( % at. )
800oC
500oC
Reactive sputtered V3Si filmsY. Zhang, V. Palmieri, W. Venturini, R. Preciso, Legnaro National Laboratory - INFN, Italy
a bSurface of two annealed samples under SEM: Grain size, (a) 0.2µm, (b) 0.5µm
Beforeannealing
After annealing
T c(K
)
Tcs of 17 K and RRR values of 18 have been
recovered by annealing in SiH4 atmosphere
No matter how good the initialsuperconducing properties of the film are
We are ready to apply the thermal diffusionmethod to 6 GHz cavities
Essence of the previous slides
Wuppertal: Nb3Sn cavity (1.5 GHz) obtained trough Snvapour phase diffusion (’90s)
Nb3Sn: Liquid solute diffusion
Linearfeedtrough
Coolingwater jacket
Furnace
Liquid Sn
Nb3Sn: Used System
Nb3Sn: Phase Diagram
Nb3Sn
<Tc phases
930°C
Nb3Sn: SEM Image
20 µm
Nb3Sn
Nb
0 2 4 6 8 10 12 14 16 18 20
0
5
10
15
20
25
30 Nb3Sn n°4: 970°C, 30min+6h
Sn a
t.%
Depth (µm)
Nb3Sn: Sn at.% vs Depth
Nb3Sn Nb
20 40 60 80 100 120 140 1600,0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1,0R
elat
ive
Inte
nsity
Angle 2θ
Nb3Sn n°4: T=970°C, 30min+6h
(200)
(210)
(211)
(222)(320)
(321)
(400)
(420)(421)
(332)(520)
(521)(440) (600)
(611)
(622)
(630)
Nb3Sn: XRD
0 2 4 6 8 10 12 14 16 18 20-0,026
-0,024
-0,022
-0,020
-0,018
-0,016
-0,014
-0,012M
' (em
u)
T (K)
Nb3Sn n°8: T=1000°C, 2h+14h
Tc = 17.3 K∆Tc = 0.1 K
Nb3Sn: A Superconductive Transition Curve
Nb
Nb3Sn
Nb3Sn Process Parameters:
T = 970°CDipping time = 1hAnnealing time = 1h
Nb3Sn Surface Treatment:
Pure HCl (55-66°C) for 15 minutes
Nb3Sn: A 6 GHz Cavity
• Liquid Sn wets the Nb surface and bulk diffusion starts
• No nucleation sites on Nb are required
• Fast growth of Nb3Sn layer due to bulk diffusion
• Uniformity of Nb3Sn film ensured and stoichiometrymantained
• We can avoid Nb-Sn low Tc phases:- manteining T > 930°C during the experiment- reducing T very fast at the end of the process
• A possible Sn outer layer has to be removed: we are ableto get rid of it by prolonged post annealing
Essence of the previous slides
6 GHz seamless cavities
obtained by the spinning technique:
And now?
We can produce a large amount of samples but it isdifficult to measure their RF resistance
• are made from scrap material
• do not need welding (even for flanges)
• are directly measured inside a Liquid He dewar
• Mechanical polishing
• Chemical polishing
3. Q Factor Measurement
• A15 obtainment
6 GHz Cavities
1. Spinning Technique
2. Surface Treatments
6 GHz Cavities: Q Factor Measurement
Nb3Sn
V
Conclusions
Nb
From scrap material and by a seamless technique
we are planning
A 6 GHz CAVITIES MASS PRODUCTION TO
INVESTIGATE A15 INTERMETALLIC COMPOUNDS
The end
A atoms form linear chains: they are parallelto the 3 crystallographic directions [100], [010], [001]
Stoichiometry ~ A3B
B
A
A15 Compounds Structure
TM
noTM
TM
Mo75Re25 Cavity (MIT 1978)
K. Agyeman, I. M. Puffer, J. A. Yasaitis and R. M. Rose, “Superconducting Mo0.75Re0.25 cavities at X-band”
Mo60Re40
A.Andreone, A.Barone, A.Di Chiara, G.Mascolo, V.Palmieri, G.Peluso, U.Scotti, 1988
Literature: Mo-Re system
6 GHz Cavities: Mechanical Polishing
6 GHz cavities: Chemical Polishing