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Surface Resistance of a 
bulk-like Nb Film 
Sarah Aull, Anne-Marie Valente-Feliciano, 
Tobias Junginger and Jens Knobloch
The Quadrupole Resonator 
sarah.aull@cern.ch 2 
• Resonant frequencies: 
400, 800, 1200 MHz 
• Same magnetic field configuration for all 
frequencies 
• Bmax ≈ 60 mT 
• Temperatures 1.8 -20 K 
• Sample: 
• 75 mm diameter 
• Equipped with a dc heater and 4 
temperature sensors 
361 mm 
Sample
sarah.aull@cern.ch 
• RF-DC-compensation 
• 푅S~ 
푃dc1−푃dc2 
푃t 
3 
Calorimetric Method 
Helium bath
• OFHC copper substrate: 
• mechanically polished 
• Electron beam welded to Nb ring (EBW 1) 
• 12 μm electro polishing 
• Rinsing with ultra pure water at 6 bar 
• Shipped to Jefferson Lab for coating 
• Shipped back to CERN, EBW to support 
structure (EBW 2) 
• Rinsing with ultra pure water at 6 bar 
• Mounted in the quadrupole resonator 
sarah.aull@cern.ch 4 
Sample Preparation 
EBW 1 
EBW 2
Deposition Conditions 
Cu substrate 
• OFHC Cu 
• Mechanical polishing + electropolishing 
• Final sulfamic acid rinse for cu passivation 
Deposition Conditions 
• ECR 
• Bake & coating temperature: 360 °C 
• Total coating time: 60’ 
Dual ion energy: 
• 184 eV for nucleation/early growth 
• 64 eV for subsequent growth 
• Hetero-epitaxial film Nb on OFHC Cu 
Typical Cu substrate 
valente@jlab.org 5
Film characterization 
Witness sample Nb/(11-20) 
Al2O3 
Tc= 9.36 ± 0.12 K 
RRR = 179 
Diffraction on Nb/Cu witness 
sample: 
EBSD IPF map and XRD pole 
figure show very good 
crystallinity and grain sizes in 
the range of the typical Cu 
substrate 
valente@jlab.org 6
Penetration Depth Measurement 
λ(0K) [nm] 
400 MHz 40 ± 2 
800 MHz 38 ± 1 
1200 MHz 38 ± 1 
Bulk-like film 
in the clean limit 
ℓ* [nm] RRR 
144 ± 20 53 ± 7 
* with λL = 32 nm 
and ξ0 = 39 nm 
sarah.aull@cern.ch 7
R(T): comparison with bulk Nb 
R(T) curve consistent with a film 
with RRR 50 and a reduced energy 
gap (might be due to strong 
oxidation) 
Rres [nΩ] Δ [K] 
400 MHz 46.6 ± 0.8 14.2 ± 0.3 
800 MHz 79 ± 2 14.8 ± 0.2 
1200 MHz 156 ± 11 15.1 ± 1 
mean 14.6 ± 0.2 
sarah.aull@cern.ch 8
• Q-Slope of Nb film is linear for 
B > 5 mT for temperatures up 
to 4 K. 
• Q-Slope of the Nb film is 
significantly stronger than for 
bulk Nb (1 order of magnitude) 
RRR is unlikely the cause for the 
strong Q-slope of Nb films. 
sarah.aull@cern.ch 9 
Q-Slope: film vs. bulk 
2.5 K 
4 K
• Thermal cycling: warm up the sample to the normal conducting state 
and cool down under different conditions. 
sarah.aull@cern.ch 10 
Thermal Cycling 
Thermal cycling does not affect the (low field) BCS contribution.
Influence of the Cooling Conditions 
• Influence on the surface resistance: Slow uniform cooling 
increases RS by more than a factor 2. 
400 MHz, 2K, 5 mT 
sarah.aull@cern.ch 11
Influence of the Cooling Conditions 
Thermal cycling acts on the Q-slope: 
The faster the cooling the flatter the slope. 
sarah.aull@cern.ch 12 
400 MHz, 2 K
Conclusions for the ECR film 
• This bulk-like Nb film shows significantly different behaviour than 
bulk Nb with the same RRR: 
• In contrary to bulk Nb: cooling fast and with a high temperature gradient 
leads to lower surface resistance. 
• Lowest surface resistance was achieved by quenching. 
• The Q-Slope of the film is much more severe than the one of bulk 
Nb. Therefore low RRR is unlikely the cause for strong Q-slopes in 
Nb film cavities. 
• The cooling conditions act on the Q-Slope, leading to better 
performance after fast cooling. 
sarah.aull@cern.ch 13
Comparison with HIPIMS coating 
• Single cell 1.3 GHz Cu cavity + EP 
• Coating by Giovanni Terenziani 
• RF Cold test by Tobias Junginger 
• For more RF results of this cavity, see: 
HIPIMS Development for 
Superconducting Cavities, Giovanni 
Terenziani & Tobias Junginger 
• Cooling rate derived from temperature 
slope at Tc 
• Lower RS for fast cooling and smaller 
temperature gradient. 
• Thermal cycling influences the Q-Slope 
as well. 
sarah.aull@cern.ch 14
Comparison with HIE Isolde 
• Quarterwave, 100 MHz 
• For more RF results, see The 
influence of cooldown 
conditions at transition 
temperature on the quality 
factor of niobium sputtered 
quarter-wave resonators, Pei 
Zhang 
• Surface resistance increases 
for larger temperature 
gradients. 
• Cooling rate has no significant 
influence on RS. 
Courtesy of Pei Zhang 15
Comparison between QPR, 1.3 GHz and HIE Isolde 
RRR Geometry Cooling Grain size 
sarah.aull@cern.ch 16 
Quadrupole 
Resonator: 
ECR 
Lower RS for 
fast cooling 
with T 
gradient 
53 disc conduction tens of 
microns 
1.3 GHz: 
HIPIMS 
Lower RS for 
fast cooling 
with small T 
gradient 
21 elliptical Bath 
cooled 
30 nm 
HIE Isolde: 
Diode 
sputtering 
Lower RS for 
small T 
gradients 
15 QWR conduction 200 nm – 
1 μm 
depending on 
thickness 
Unknown 
Influence of grain 
size 
Influence of 
geometry 
Thermal currents 
Influence of 
stress 
Oxidation 
Roughness 
…
Conclusions for Nb films 
• As for bulk Nb: The cooling conditions, speed and/or spatial 
gradient, influence the RF performance. 
• Different film projects are difficult to compare due to different 
coating techniques and geometries. 
• Optimum cooling procedure to minimize the low field RS is 
accompanied by a flattened Q-Slope. 
• Further conclusions require dedicated experiments, where 
spatial and temporal gradients and thermal currents can be 
controlled independently. 
sarah.aull@cern.ch 17
Backup 
sarah.aull@cern.ch 18
Electron Cyclotron Resonance 
No working gas 
Ions produced in vacuum 
Singly charged ions 64eV 
Controllable deposition energy with Bias voltage 
Excellent bonding 
No macro particles 
Good conformality 
Generation of plasma 
3 essential components: 
Neutral Nb vapor 
RF power (@ 2.45GHz) 
Static B  ERF with ECR condition 
eB 
m 
 

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Sarah aull secondary electron yield of srf materials

  • 1. Surface Resistance of a bulk-like Nb Film Sarah Aull, Anne-Marie Valente-Feliciano, Tobias Junginger and Jens Knobloch
  • 2. The Quadrupole Resonator sarah.aull@cern.ch 2 • Resonant frequencies: 400, 800, 1200 MHz • Same magnetic field configuration for all frequencies • Bmax ≈ 60 mT • Temperatures 1.8 -20 K • Sample: • 75 mm diameter • Equipped with a dc heater and 4 temperature sensors 361 mm Sample
  • 3. sarah.aull@cern.ch • RF-DC-compensation • 푅S~ 푃dc1−푃dc2 푃t 3 Calorimetric Method Helium bath
  • 4. • OFHC copper substrate: • mechanically polished • Electron beam welded to Nb ring (EBW 1) • 12 μm electro polishing • Rinsing with ultra pure water at 6 bar • Shipped to Jefferson Lab for coating • Shipped back to CERN, EBW to support structure (EBW 2) • Rinsing with ultra pure water at 6 bar • Mounted in the quadrupole resonator sarah.aull@cern.ch 4 Sample Preparation EBW 1 EBW 2
  • 5. Deposition Conditions Cu substrate • OFHC Cu • Mechanical polishing + electropolishing • Final sulfamic acid rinse for cu passivation Deposition Conditions • ECR • Bake & coating temperature: 360 °C • Total coating time: 60’ Dual ion energy: • 184 eV for nucleation/early growth • 64 eV for subsequent growth • Hetero-epitaxial film Nb on OFHC Cu Typical Cu substrate valente@jlab.org 5
  • 6. Film characterization Witness sample Nb/(11-20) Al2O3 Tc= 9.36 ± 0.12 K RRR = 179 Diffraction on Nb/Cu witness sample: EBSD IPF map and XRD pole figure show very good crystallinity and grain sizes in the range of the typical Cu substrate valente@jlab.org 6
  • 7. Penetration Depth Measurement λ(0K) [nm] 400 MHz 40 ± 2 800 MHz 38 ± 1 1200 MHz 38 ± 1 Bulk-like film in the clean limit ℓ* [nm] RRR 144 ± 20 53 ± 7 * with λL = 32 nm and ξ0 = 39 nm sarah.aull@cern.ch 7
  • 8. R(T): comparison with bulk Nb R(T) curve consistent with a film with RRR 50 and a reduced energy gap (might be due to strong oxidation) Rres [nΩ] Δ [K] 400 MHz 46.6 ± 0.8 14.2 ± 0.3 800 MHz 79 ± 2 14.8 ± 0.2 1200 MHz 156 ± 11 15.1 ± 1 mean 14.6 ± 0.2 sarah.aull@cern.ch 8
  • 9. • Q-Slope of Nb film is linear for B > 5 mT for temperatures up to 4 K. • Q-Slope of the Nb film is significantly stronger than for bulk Nb (1 order of magnitude) RRR is unlikely the cause for the strong Q-slope of Nb films. sarah.aull@cern.ch 9 Q-Slope: film vs. bulk 2.5 K 4 K
  • 10. • Thermal cycling: warm up the sample to the normal conducting state and cool down under different conditions. sarah.aull@cern.ch 10 Thermal Cycling Thermal cycling does not affect the (low field) BCS contribution.
  • 11. Influence of the Cooling Conditions • Influence on the surface resistance: Slow uniform cooling increases RS by more than a factor 2. 400 MHz, 2K, 5 mT sarah.aull@cern.ch 11
  • 12. Influence of the Cooling Conditions Thermal cycling acts on the Q-slope: The faster the cooling the flatter the slope. sarah.aull@cern.ch 12 400 MHz, 2 K
  • 13. Conclusions for the ECR film • This bulk-like Nb film shows significantly different behaviour than bulk Nb with the same RRR: • In contrary to bulk Nb: cooling fast and with a high temperature gradient leads to lower surface resistance. • Lowest surface resistance was achieved by quenching. • The Q-Slope of the film is much more severe than the one of bulk Nb. Therefore low RRR is unlikely the cause for strong Q-slopes in Nb film cavities. • The cooling conditions act on the Q-Slope, leading to better performance after fast cooling. sarah.aull@cern.ch 13
  • 14. Comparison with HIPIMS coating • Single cell 1.3 GHz Cu cavity + EP • Coating by Giovanni Terenziani • RF Cold test by Tobias Junginger • For more RF results of this cavity, see: HIPIMS Development for Superconducting Cavities, Giovanni Terenziani & Tobias Junginger • Cooling rate derived from temperature slope at Tc • Lower RS for fast cooling and smaller temperature gradient. • Thermal cycling influences the Q-Slope as well. sarah.aull@cern.ch 14
  • 15. Comparison with HIE Isolde • Quarterwave, 100 MHz • For more RF results, see The influence of cooldown conditions at transition temperature on the quality factor of niobium sputtered quarter-wave resonators, Pei Zhang • Surface resistance increases for larger temperature gradients. • Cooling rate has no significant influence on RS. Courtesy of Pei Zhang 15
  • 16. Comparison between QPR, 1.3 GHz and HIE Isolde RRR Geometry Cooling Grain size sarah.aull@cern.ch 16 Quadrupole Resonator: ECR Lower RS for fast cooling with T gradient 53 disc conduction tens of microns 1.3 GHz: HIPIMS Lower RS for fast cooling with small T gradient 21 elliptical Bath cooled 30 nm HIE Isolde: Diode sputtering Lower RS for small T gradients 15 QWR conduction 200 nm – 1 μm depending on thickness Unknown Influence of grain size Influence of geometry Thermal currents Influence of stress Oxidation Roughness …
  • 17. Conclusions for Nb films • As for bulk Nb: The cooling conditions, speed and/or spatial gradient, influence the RF performance. • Different film projects are difficult to compare due to different coating techniques and geometries. • Optimum cooling procedure to minimize the low field RS is accompanied by a flattened Q-Slope. • Further conclusions require dedicated experiments, where spatial and temporal gradients and thermal currents can be controlled independently. sarah.aull@cern.ch 17
  • 19. Electron Cyclotron Resonance No working gas Ions produced in vacuum Singly charged ions 64eV Controllable deposition energy with Bias voltage Excellent bonding No macro particles Good conformality Generation of plasma 3 essential components: Neutral Nb vapor RF power (@ 2.45GHz) Static B  ERF with ECR condition eB m  