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"Presence of residual Tin drops in Thermally diffused Nb3Sn" Authors:        Konstantin Atroshchenko Antonio Alessandro Rossi Supervisor:   prof. Enzo Palmieri
Liquid tin diffusion is a method of obtaining the superconductive A15 Nb3Sncoating over the 6 GHz cavities or other substrates. A bulk Nb 6 GHz cavity is introduced into molten Sn (dipping step) and after it follows the heat treatment (annealing step).  Advantages of the liquid Tin diffusion method  ,[object Object]
    uniformity of the film (stoichiometrically);
    can be used for covering surface of wide and complex  shaped substrates (!).
we don't need to manipulate dangerous substances as SnCl2to create a nucleation centers, and the diffusion process is considerably faster,[object Object]
Experimental stand linear feedthrough ,[object Object],top chamber flanges pumping cooling  water upper furnace ,[object Object],cavity lower furnace crucible with liquid Tin
Problems of the method Problem: ,[object Object],Problem:  ,[object Object]
Diffusion of contaminations through the wall of the chamber at high temperaturesexternal  furnace cavity droplets  of Tin vacuum chamber
Residual Tin drops on the internal and external surface of the cavity External surface  Internal surface  Sn Nb3Sn Sn
The L - samples 15 For the experiment was designed the L-samples, which imitates the shape of the cavity. Samples is made of Niobium.   3 50 10
Basic surface treatment (for all samples) 1.   Mechanical treatment All samples have been lapped using abrasive papers to reduce the residual roughness after machining. 2.   Basic chemical treatments ,[object Object]
washing in deionized water with ultrasonic
washing with deionized water
drying with nitrogen
BCP in the solution:  HF/HNO3/H3PO4 = 1/1/2
washing with deionized water
drying with nitrogen,[object Object]
Glow Discharge. Results. Flange Ceramic  tube  Sample After dipping and annealing @ 1000oC Horizontally fixed sample Nb wire Glow discharge. View from the  bottom window After glow discharge

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Residual Tin Removal Methods

  • 1. "Presence of residual Tin drops in Thermally diffused Nb3Sn" Authors: Konstantin Atroshchenko Antonio Alessandro Rossi Supervisor: prof. Enzo Palmieri
  • 2.
  • 3. uniformity of the film (stoichiometrically);
  • 4. can be used for covering surface of wide and complex shaped substrates (!).
  • 5.
  • 6.
  • 7.
  • 8. Diffusion of contaminations through the wall of the chamber at high temperaturesexternal furnace cavity droplets of Tin vacuum chamber
  • 9. Residual Tin drops on the internal and external surface of the cavity External surface Internal surface Sn Nb3Sn Sn
  • 10. The L - samples 15 For the experiment was designed the L-samples, which imitates the shape of the cavity. Samples is made of Niobium. 3 50 10
  • 11.
  • 12. washing in deionized water with ultrasonic
  • 15. BCP in the solution: HF/HNO3/H3PO4 = 1/1/2
  • 17.
  • 18. Glow Discharge. Results. Flange Ceramic tube Sample After dipping and annealing @ 1000oC Horizontally fixed sample Nb wire Glow discharge. View from the bottom window After glow discharge
  • 19. Preparing the surface. Anodization Procedure: Ultrasonic + Rodaclean 60 min sample Clean with acetone Ammonium citrate Clean with alcohol BCP 10 min To the power supply After anodization After dipping and annealing @ 1000oC Anodization in ammonium citrate. V = 20V Annealing. 4 hours. T = 1000OC
  • 20. Preparing the surface. Chemical etching Procedure: Ultrasonic + Rodaclean 60 min Clean with acetone Clean with alcohol Chemical etching HNO3 : HF = 1 : 1 After annealing After etching
  • 21. Comparison of external resistive and internal heaters
  • 22. Internal heater high temperature annealing The cross-section of the system: Linear feedthrough L - samples Hot zone heater Cold zone Vacuum chamber Pumping out
  • 23. Vacuum Chamber Whole – metal valve Vacuum chamber Pumping control unit Gate switch baking control unit Temperature control unit
  • 24. Comparison of annealing at 1000OC and 1300OC annealing at 1300OC for 5 minutes annealing at 1000OC for 4 hours Just BSP anodization etching glow discharge
  • 25.
  • 26. SEM measurements
  • 27. Profilometric measurements
  • 28. Covering of the Nb 6 GHz cavities;
  • 29.
  • 30. Phase diagram of Nb - Sn
  • 31. Short theoretical part The theoretical explanation of the process is basis on the Fick’s first law In two or more dimensions we must use the operator, which generalizes the first derivative, obtaining
  • 32.
  • 34. maximum rf - power: 5 kW
  • 35. process temperature: 1200 – 1500OCfeedthrough (Nb) wave – guide coil samples vacuum chamber sample after annealing
  • 36. High – temperature annealing heater
  • 37. Heating of the 6 GHz cavity