ep on small samples at fermilab - cornell university · ep on small samples at fermilab c. boffo,...

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EP on Small Samples at Fermilab C. Boffo, P. Bauer, T. Reid, FNAL, Batavia, IL 60510, U.S.A. R. Geng, Cornell University, Ithaca, NY, U.S.A. Being the electropolishing process (EP) worldwide considered an essential step in the processing of high gradient SRF cavities, studies on EP of small samples has been started at Fermilab as part of the SRF materials R&D program. A simple bench top setup has been developed to understand the basic variables affecting the EP. In addition a setup for vertical EP of half cells, based on the Cornell design, has been used and one for dumbbells has been designed and tested. Results and findings are reported. Small Samples Half Cells in Vertical Setup Next Steps Setup and Model of Half cell vertical EP Models of Vertical EP on Dumbbells EP on 3.9 GHz half cells has been performed adopting the vertical setup developed at Cornell University. During EP the fixture is placed in a chemical hood inside a secondary container. The secondary container is filled with water and ice to control temperature. Both the temperature of acid and water are monitored. The agitation of the acid is performed via Teflon coated magnetic stir bar. The same DAQ as for small samples is used. The above table shows the localized material removal during EP in different positions of the half cell along two orthogonal radii. These measurements where performed using an ultrasonic thickness measurement instrument. A fixture enabling to EP 3.9 GHz dumbbells in vertical position is being tested. The goal of this effort is to fabricate a 3 cells cavity using dumbbells and half cells electro polished before the final welding. Possible solutions for horizontal EP of full 1.3 GHz cavities are being investigated. Alternative acid mixes for EP and BCP will be investigated. Etch ( µ m) R a (um) Treatment Sample # 24 1.27 3rd BCP 29 0.95 2nd BCP 26 0.63 1st BCP - 0.45 HT 57 0.48 EP - 0.83 RAW B 25 1.26 3rd BCP 25 1.06 2nd BCP 23 0.67 1st BCP - 0.31 HT 77 0.31 EP - 0.79 RAW A Etch ( µ m) R a (um) Treatment Sample # 26 0.60 3rd EP 59 2nd EP 146 1st EP 3 191 1.8134 BCP Etch ( µ m) R a (um) Treatment Sample # 13 8 10 10 15 5 10 13 EP 1 [ µ m] 8 2.681 3 15 2.676 4 18 2.726 5 13 2.737 6 18 2.668 7 10 2.655 8 15 2.739 2 15 2.734 1 EP 2 [ µ m] Initial [mm] Point Stir Bar PTFE Half Cell 5 8 6 7 1 4 3 2 99.95 % Al Cathode Agitator Anode Connection 99.95 % Al Cathode PTFE Net Temperature dependence of Oscillation Frequency in EP of FNAL 3.9 GHz Half Cell 0.25 0.3 0.35 0.4 0.45 0.5 0.55 0.6 30 31 32 33 34 35 36 37 38 39 40 Temperature [C] Frequency [Hz] The EP setup for small samples is very simple and allows to have a good control on all fundamental parameters. Voltage drop, current, temperature of acid and temperature of water are monitored using in parallel: a strip chart analog recorder and a USB NI DAQ connected to a laptop. Data are acquired using a NI LabView custom application. The most complicated parameter to quantify is the acid agitation obtained with a magnetic stir bar . Current voltage characteristics as a function of temperature and characterization of the current oscillations have been studied. Software based 3D reconstruction and profilometry are used to quantitatively characterize the effect of BCP, EP, and Heat treatments on the surface topography of Nb. Two SEM images of the same area, obtained at different angles, are used for a 3D reconstruction. Profilometry performed on this reconstructed images may allow better resolution with respect to mechanical measurements but the technique needs to be carefully debugged first. Attempts of using a commercial software are presented Nb Surface profiles using Alicona MEX Systematic studies of the surface roughness of small samples has been performed. A first set of samples have been BCP etched and later EP has been performed in successive steps A second set of samples have been EP and later BCP etched in successive steps. The average roughness have been measured using a Taylor Hobson Talysurf Intra device equipped with a 2 µm radius diamond chisel EP SEM and Profile BCP SEM and Profile

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Page 1: EP on Small Samples at Fermilab - Cornell University · EP on Small Samples at Fermilab C. Boffo, P. Bauer, T. Reid, FNAL, Batavia, IL 60510, U.S.A. R. Geng, Cornell University, Ithaca,

EP on Small Samples at Fermilab C. Boffo, P. Bauer, T. Reid, FNAL, Batavia, IL 60510, U.S.A. R. Geng, Cornell University, Ithaca, NY, U.S.A.

Being the electropolishing process (EP) worldwide considered an essential step in the processing of high gradient SRF cavities, studies on EP of small samples has been started at Fermilab as part of the SRF materials R&D program.A simple bench top setup has been developed to understand the basic variables affecting the EP. In addition a setup for vertical EP of half cells, based on the Cornell design, has been used and one for dumbbells has been designed and tested. Results and findings arereported.

Small Samples Half Cells in Vertical Setup

Next Steps

Setup and Model of Half cell vertical EP

Models of Vertical EP on Dumbbells

EP on 3.9 GHz half cells has been performed adopting the vertical setup developed at Cornell University. During EP the fixture is placed in a chemical hood inside a secondary container. The secondary container is filled with water and ice to control temperature. Both the temperature of acid and water are monitored. The agitation of the acid is performed via Teflon coated magnetic stir bar. The same DAQ as for small samples is used. The above table shows the localized material removal during EP in different positions of the half cell along two orthogonal radii. These measurements where performed using an ultrasonic thickness measurement instrument.

A fixture enabling to EP 3.9 GHz dumbbells in vertical position is being tested. The goal of this effort is to fabricate a 3 cells cavity using dumbbells and half cells electro polished before the final welding. Possible solutions for horizontal EP of full 1.3 GHz cavities are being investigated.Alternative acid mixes for EP and BCP will be investigated.

Etch (µm)Ra (um)TreatmentSample #

241.273rd BCP290.952nd BCP260.631st BCP-0.45HT

570.48EP-0.83RAW

B

251.263rd BCP251.062nd BCP230.671st BCP-0.31HT

770.31EP-0.79RAW

A

Etch (µm)Ra (um)TreatmentSample #

260.603rd EP592nd EP1461st EP3

1911.8134BCPEtch (µm)Ra (um)TreatmentSample #

13810101551013

EP 1 [µm]

82.6813152.6764182.7265132.7376182.6687102.6558

152.7392152.7341

EP 2 [µm]Initial [mm]Point

Stir Bar

PTFE Half Cell

586 7

1

43

2

99.95 % Al Cathode

Agitator

Anode Connection

99.95 % Al Cathode

PTFE Net

Temperature dependence of Oscillation Frequency in EP of FNAL 3.9 GHz Half Cell

0.25

0.3

0.35

0.4

0.45

0.5

0.55

0.6

30 31 32 33 34 35 36 37 38 39 40

Temperature [C]

Freq

uenc

y [H

z]

The EP setup for small samples is very simple and allows to have a good control on all fundamental parameters. Voltage drop, current, temperature of acid and temperature of water are monitored using in parallel: a strip chart analog recorder and a USB NI DAQ connected to a laptop. Data are acquired using a NI LabView custom application. The most complicated parameter to quantify is the acid agitation obtained with a magnetic stir bar .Current voltage characteristics as a function of temperature and characterization of the current oscillations have been studied.

Software based 3D reconstruction and profilometry are used to quantitatively characterize the effect of BCP, EP, and Heat treatments on the surface topography of Nb. Two SEM images of the same area, obtained at different angles, are used for a 3D reconstruction. Profilometry performed on this reconstructed images may allow better resolution with respect to mechanical measurements but the technique needs to be carefully debugged first. Attempts of using a commercial software are presented

Nb Surface profiles using Alicona MEX

Systematic studies of the surface roughness of small samples has been performed.A first set of samples have been BCP etched and later EP has been performed in successive steps A second set of samples have been EP and later BCP etched in successive steps.

The average roughness have been measured using a Taylor Hobson Talysurf Intra device equipped with a 2 µm radius diamond chisel

EP SEM and Profile

BCP SEM and Profile