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NATIONAL INSTITUTE OF NUCLEAR PHYSICS 
PADOVA UNIVERSITY 
Preparation of Nb3(Ga,Al) 
superconductors by Electromagnetic 
Induction Heating 
Camacho A., Rossi A., Palmieri V. 
Sixth International Workshop on Thin Films and New Ideas for RF Superconductivity
Outline 
• Introduction of the common techniques used to prepare binary and 
ternary superconducting A15 compounds. 
• Electromagnetic Induction Heating Technique. 
• Experimental procedure: 
• Samples preparation. 
• Heat Treatment Performed. 
• Validation of the technique according superconducting properties and 
quality of A15 phase on samples. 
• Application of our technique on 6 GHz niobium cavities. 
• Conclusions.
Introduction 
• Common techniques used to prepare A15 superconducting phase: 
Arc-melting process, chemical vapor deposition (CVD), sputtering, 
etc. 
• More specialized techniques such as: 
• Melt-spin quenching technique: Nb3Ga  20.0K, V3Ga 
15.0K, and Nb3Al  18.4K reported by Clemente [1] 
[1] Clemente,“Superconducting properties of A15 compounds prepared by melt-spin quenching“
EM- Induction Heating 
 Rapid heating 
 High temperatures during annealing process (~3000 °C) 
 Vacuumless 
 Self-heating of the sample 
 Short time of treatment 
 Clean quartz chamber 
 Economic system
Application on 6 GHz niobium Cavities 
A15 compounds by 
EM-IH technique 
6 GHz Nb Cavities
EM- Induction Heating System 
Work head 
15 KW 
Power 
supply 
(250-3000)ºC 
Pyrometer 
Flange 
Quartz 
tube 
Flange 
Argon 
or 
Helium 
Low overpressure 
Exhaust gases 
Coil 
Input gas 
Cavity or Sample
Experimental Procedure 
Before annealing the samples 
(20x10x5) mm 
Chemical Treatment 
BCP solution: 
HF/HNO3/H3PO4 = 1:1:2
Experimental Procedure 
How? 
• Binary compounds Configuration I: 
 Liquid Gallium (99.9% pure) 
 Aluminum Foil (99% pure) 
• Ternary compounds  Configuration I 
and II: 
 Paste: liq. Ga+ Al foil 
Configuration I 
Configuration II
Heat Treatment 
Changing the voltage 
and time 
Rapid heating, quenching and transformation
Validation of the EM-IH Technique 
Materials Number of samples Total 
Nb-Ga 10 
Nb-Al 6 61 
Nb-Al-Ga 45 
Inductive 
Measurement 
Tc
Binary Compounds 
Heat treatment for 10 minutes, changing the temperature from 1500 °C up to 1800 °C
Binary Compounds 
• All the Tc are near to 12 K, an average of 3 K above of niobium transition 
(9 K). 
• The difficult to synthetize binary A15 compounds (Nb3Ga and Nb3Al) is 
related to the competition from more stable phases, such as s phases 
(Nb2Al and Nb5Ga3) and a-Nb phases (solid solution in bcc structure of 
niobium). 
• Samples annealed that not reach temperatures higher than 1500ºC, only 
Nb superconducting transition was evidenced. 
• The results suggest that the annealing process for 10 minutes at high 
temperatures degrades the superconducting phase initially formed
Nb3Ga Nb3Al 
Lattice parameter of 5.1809 Å, very close to 
the standard lattice parameter, 5.1800 Å 
Lattice parameter of 5.2141 Å, much 
higher than the standard value, 5.1780 Å.
From our first attempt of A15 
phase, we concluded... 
1. Critical temperature results suggest higher diffusion of 
gallium atoms than aluminum atoms on niobium 
samples at the same heating conditions (corrosive 
property of gallium) 
2. Wettability problems with liquid gallium which make 
the preparation of the samples before the heat 
treatment difficult 
3. Very short time of heat treatment is necessary 
TERNARY COMPOUNDS!!! Nb-Al-Ga
Ternary Compounds 
Tc= (18±0.35)K 
1 
Heat treatment for ~1 minute, changing the temperature from 1420 °C up to 2000 °C
High Tc and sharp superconducting 
transition 
• Direct transformation of A15 phase from high temperatures of 
niobium samples. 
• Ternary compound seems to stabilize the A15 phase.
Ternary Compounds 
2 
Heat treatment for ~1 minute, changing the temperature from 1420 °C up to 2000 °C
Broad superconducting transitions 
• Gallium/ aluminum evaporate. 
• Less control of the stoichiometry. 
• Further studies are required in order to 
establish a relation of the quantity of aluminum/ 
gallium evaporated.
(210) 
(200) 
(310) 
(320) 
(211) 
X-ray diffraction in the planes: 
• (321) Nb3Ga 
• (110) Nb3Al 
were not observed 
Lattice parameter: 5.1904 Å 
a-Nb3Ga< a-Nb3(Al,Ga)< a-Nb3Al
Profile temperature vs time 
Heating rate: 
90 [˚C/s] 
Cooling rate: 
50 [˚C/s]
Results Microstructure of Nb-Ga-Al_1 sample 
Niobium x Nb-Al-Ga 
Niobium Nb-Al-Ga 
Crack 
x 
Element wt% At.% 
Nb 82±1 66±1 
Ga 11,3±0,9 12,1±0,9 
O 1,9±0,1 9,0±0,6 
Al 4,7±0,2 12,9±0,4 
73% at. Nb, 13.3% at. Ga and 14.2% at. Al.  A15 and A2
Results 
Microstructure of Nb-Ga-Al_1 sample 
Niobium Nb-Al-Ga
Results Nb-Al-Ga Samples 
Microstructure of Nb-Ga-Al_1 sample 
Niobium x 
x 
Nb-Al-Ga Niobium Nb-Al-Ga 
Nb-Al-Ga Niobium
Results 
Mapping that shows the interface between niobium and 
superconducting layer 
Total Counts X-Rays 
Element Color Smin Smax 
O K Red 11 99 
Ga L Green 17 405 
Al K Blue 19 296 
Nb L Yellow 151 2805 
Ga K Purple 21 366
Nb (L) Ga (K) Al (K) 
Ga (L)-Nb (L) Al (K)-Nb (L) 
O (K)- Nb (L) 
Ga (L)-Al (K) Ga (L)-Al (K)-Nb (L) Ga (L)-Al (K)-Nb (L)- O (K)
6 GHz niobium Cavities
Experimental Procedure 
Before Coating: 1. Centrifugal Tumbling
Experimental Procedure 
Before Coating: 2. Chemical Treatment, BCP solution 
Before Coating: 3. High Pressure Water Rising
Experimental Procedure 
Rotator 
Liquid Gallium
Experimental Procedure 
Yttria- stabilized Zirconium oxide 
Inside Liq. gallium 
or paste with
Cavities Measurements 
Sample Time [min.] Annealing Temperature, Max. [°C] Notes 
1 1,3 2000 Melted 
2 14,4 1731 Cavity with a small hole. 
3 2,2 1770 Melted 
4 3,0 1200 Normal conductor 
5 
10,0 1091 Normal conductor 
6 
6,1 2031 Normal conductor 
7 
1,4 1830 Normal conductor
Experimental Procedure
Conclusions 
Direct transition of superconducting phase from high temperatures 
using E-M induction heating. 
The temperature of the samples are very sensitive by changing voltage 
and time. 
Nb+Al+Ga stabilized the A15 superconducting phase. 
The best configuration is niobium+aluminum/gallium+niobium which 
avoid the evaporation of gallium and aluminum at high temperatures  
more control of the stoichiometry  SHARP HIGH SC TRANSITION
Thanks for your attention

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Andrea maria camacho romero - preparation of nb3 gaal superconductors

  • 1. NATIONAL INSTITUTE OF NUCLEAR PHYSICS PADOVA UNIVERSITY Preparation of Nb3(Ga,Al) superconductors by Electromagnetic Induction Heating Camacho A., Rossi A., Palmieri V. Sixth International Workshop on Thin Films and New Ideas for RF Superconductivity
  • 2. Outline • Introduction of the common techniques used to prepare binary and ternary superconducting A15 compounds. • Electromagnetic Induction Heating Technique. • Experimental procedure: • Samples preparation. • Heat Treatment Performed. • Validation of the technique according superconducting properties and quality of A15 phase on samples. • Application of our technique on 6 GHz niobium cavities. • Conclusions.
  • 3. Introduction • Common techniques used to prepare A15 superconducting phase: Arc-melting process, chemical vapor deposition (CVD), sputtering, etc. • More specialized techniques such as: • Melt-spin quenching technique: Nb3Ga  20.0K, V3Ga 15.0K, and Nb3Al  18.4K reported by Clemente [1] [1] Clemente,“Superconducting properties of A15 compounds prepared by melt-spin quenching“
  • 4. EM- Induction Heating  Rapid heating  High temperatures during annealing process (~3000 °C)  Vacuumless  Self-heating of the sample  Short time of treatment  Clean quartz chamber  Economic system
  • 5. Application on 6 GHz niobium Cavities A15 compounds by EM-IH technique 6 GHz Nb Cavities
  • 6. EM- Induction Heating System Work head 15 KW Power supply (250-3000)ºC Pyrometer Flange Quartz tube Flange Argon or Helium Low overpressure Exhaust gases Coil Input gas Cavity or Sample
  • 7. Experimental Procedure Before annealing the samples (20x10x5) mm Chemical Treatment BCP solution: HF/HNO3/H3PO4 = 1:1:2
  • 8. Experimental Procedure How? • Binary compounds Configuration I:  Liquid Gallium (99.9% pure)  Aluminum Foil (99% pure) • Ternary compounds  Configuration I and II:  Paste: liq. Ga+ Al foil Configuration I Configuration II
  • 9. Heat Treatment Changing the voltage and time Rapid heating, quenching and transformation
  • 10. Validation of the EM-IH Technique Materials Number of samples Total Nb-Ga 10 Nb-Al 6 61 Nb-Al-Ga 45 Inductive Measurement Tc
  • 11. Binary Compounds Heat treatment for 10 minutes, changing the temperature from 1500 °C up to 1800 °C
  • 12. Binary Compounds • All the Tc are near to 12 K, an average of 3 K above of niobium transition (9 K). • The difficult to synthetize binary A15 compounds (Nb3Ga and Nb3Al) is related to the competition from more stable phases, such as s phases (Nb2Al and Nb5Ga3) and a-Nb phases (solid solution in bcc structure of niobium). • Samples annealed that not reach temperatures higher than 1500ºC, only Nb superconducting transition was evidenced. • The results suggest that the annealing process for 10 minutes at high temperatures degrades the superconducting phase initially formed
  • 13. Nb3Ga Nb3Al Lattice parameter of 5.1809 Å, very close to the standard lattice parameter, 5.1800 Å Lattice parameter of 5.2141 Å, much higher than the standard value, 5.1780 Å.
  • 14. From our first attempt of A15 phase, we concluded... 1. Critical temperature results suggest higher diffusion of gallium atoms than aluminum atoms on niobium samples at the same heating conditions (corrosive property of gallium) 2. Wettability problems with liquid gallium which make the preparation of the samples before the heat treatment difficult 3. Very short time of heat treatment is necessary TERNARY COMPOUNDS!!! Nb-Al-Ga
  • 15. Ternary Compounds Tc= (18±0.35)K 1 Heat treatment for ~1 minute, changing the temperature from 1420 °C up to 2000 °C
  • 16. High Tc and sharp superconducting transition • Direct transformation of A15 phase from high temperatures of niobium samples. • Ternary compound seems to stabilize the A15 phase.
  • 17. Ternary Compounds 2 Heat treatment for ~1 minute, changing the temperature from 1420 °C up to 2000 °C
  • 18. Broad superconducting transitions • Gallium/ aluminum evaporate. • Less control of the stoichiometry. • Further studies are required in order to establish a relation of the quantity of aluminum/ gallium evaporated.
  • 19. (210) (200) (310) (320) (211) X-ray diffraction in the planes: • (321) Nb3Ga • (110) Nb3Al were not observed Lattice parameter: 5.1904 Å a-Nb3Ga< a-Nb3(Al,Ga)< a-Nb3Al
  • 20. Profile temperature vs time Heating rate: 90 [˚C/s] Cooling rate: 50 [˚C/s]
  • 21. Results Microstructure of Nb-Ga-Al_1 sample Niobium x Nb-Al-Ga Niobium Nb-Al-Ga Crack x Element wt% At.% Nb 82±1 66±1 Ga 11,3±0,9 12,1±0,9 O 1,9±0,1 9,0±0,6 Al 4,7±0,2 12,9±0,4 73% at. Nb, 13.3% at. Ga and 14.2% at. Al.  A15 and A2
  • 22. Results Microstructure of Nb-Ga-Al_1 sample Niobium Nb-Al-Ga
  • 23. Results Nb-Al-Ga Samples Microstructure of Nb-Ga-Al_1 sample Niobium x x Nb-Al-Ga Niobium Nb-Al-Ga Nb-Al-Ga Niobium
  • 24. Results Mapping that shows the interface between niobium and superconducting layer Total Counts X-Rays Element Color Smin Smax O K Red 11 99 Ga L Green 17 405 Al K Blue 19 296 Nb L Yellow 151 2805 Ga K Purple 21 366
  • 25. Nb (L) Ga (K) Al (K) Ga (L)-Nb (L) Al (K)-Nb (L) O (K)- Nb (L) Ga (L)-Al (K) Ga (L)-Al (K)-Nb (L) Ga (L)-Al (K)-Nb (L)- O (K)
  • 26. 6 GHz niobium Cavities
  • 27. Experimental Procedure Before Coating: 1. Centrifugal Tumbling
  • 28. Experimental Procedure Before Coating: 2. Chemical Treatment, BCP solution Before Coating: 3. High Pressure Water Rising
  • 30. Experimental Procedure Yttria- stabilized Zirconium oxide Inside Liq. gallium or paste with
  • 31. Cavities Measurements Sample Time [min.] Annealing Temperature, Max. [°C] Notes 1 1,3 2000 Melted 2 14,4 1731 Cavity with a small hole. 3 2,2 1770 Melted 4 3,0 1200 Normal conductor 5 10,0 1091 Normal conductor 6 6,1 2031 Normal conductor 7 1,4 1830 Normal conductor
  • 33. Conclusions Direct transition of superconducting phase from high temperatures using E-M induction heating. The temperature of the samples are very sensitive by changing voltage and time. Nb+Al+Ga stabilized the A15 superconducting phase. The best configuration is niobium+aluminum/gallium+niobium which avoid the evaporation of gallium and aluminum at high temperatures  more control of the stoichiometry  SHARP HIGH SC TRANSITION
  • 34. Thanks for your attention