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Copper Electroforming
        Status Report

             Silvia Borjabad
   7th JRA-1 Meeting   Zaragoza (November 2007)
OUTLINE

                 Copper Electroforming Process

                 Review of objectives and work progress
                 Summary and prospects




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Copper Electroforming Process

Electroforming is a method of producing pieces by the deposition
of a metal onto a mold (mandrel) which is subsequently removed

                              Copper Electroforming Overview
            ENGINE


                                                               • High-purity copper parts
      TANK
                                                               • Accurate surface
                                          FILTER                 reproduction
                                                               • Underground process
                                                               • Chemical & electrolitic
                                                                 improvements


             CuSO 4                                    PUMP
             H 2SO4


S. Borjabad 7th JRA-1 Zaragoza Nov´07
Copper Electroforming Process
                             Process Parameters & Key Elements

   • Mandrel turns during the whole process
     producing a homogeneous deposition
                                                      Constituents of the Electrolyte
   • Electrolyte circulates with continuous
                                                       Constituent         Concentration
     filtration to eliminate impurities
   • Covered bath avoids air and dust                 CuSO4 . 5H2O              188 g/l

     contamination                                        H2SO4                  75 g/l

   • Plating is done over polished and cleaned             HCl                  30 mg/l
     stainless steel mandrels with the same             Thiourea                3 mg/l
     shape of the relevant copper parts
                                                       (Brodzinski et al.,A292 (1990) 337)
   • H2SO4 improves the electric conductivity
   • HCl and Thiourea affect copper crystal
     nucleation and grain size

S. Borjabad 7th JRA-1 Zaragoza Nov´07
Copper Electroforming Process
                                           Electroforming Set-Up

                                        Voltage Supply
                                                                            Electronic
                                                                          Control System
                                                                           • Rotation Speed & Direction
                     Electrolitic Bath
                                                                           • Plating modes
     • Electrolyte circulation
     • Inert cover gas (N2)


                                                          Temperature
                                                         and pH sensors
                                                                           • Temperature & pH sensors
                                                                           • Parameters DAQ system
                               Filter and Pump




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress



        Electroforming process parameter tuning
        Electroformed copper parts with complex geometry
        Monitorization of parameters during the electroforming process
        Radiopurity measurements of electroformed copper parts
        Chemical & electrolytic improvements
        Electroforming in steps to fabricate cryostat copper components




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress
                       Electroforming Process Parameter Tuning

                                        Smooth surface
                          Goals         Homogeneous copper distribution
                                        Without periodic machining process

         Parameters: Current Density, Speed Rotation and Direction Rotation




                                   Optimum parameters: 3 A/dm2, 2 rev/s, forward-reverse rotation


S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress
              Electroformed copper parts with complex geometry
   • Hexagonal & cylindrical electroformed copper parts

                                                                              • Smooth
    Isolated areas                                                              surface
     with Teflon,
      parafine or                                                             • Accurate
       silicone                                                                 surface
                                                                                reproduction
                                                                                (corners)
                                                    1.5 mm of thickness


   • Electroformed copper part for PMT encapsulation (collaboration ANAIS)

                                                                          • Smooth surface
   Isolated
                                                                               h
                                                                           wit gress
                                                                          • Homogeneous
  areas with
                                                                         s o
                                                                      est distribution
    Teflon
                                                                       t     rp
                                                                 e  ing g in Final machining
                                                                   r in •
                                                            old rm
                                                          S fo                process
                                                              r o
               Complex mandrel          Auxiliary
                                                       el ect              1.5-2 mm of thickness
                                         anode
S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress



        Electroforming process parameter tuning
        Electroformed copper parts with complex geometry
        Monitorization of parameters during the electroforming process
        Radiopurity measurements of electroformed copper parts
        Chemical & electrolytic improvements
        Electroforming in steps to fabricate cryostat copper components




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress
            Parameters monitorization during the electroforming

                             Current (I)
 Electroforming                                             Evolution during the process
   Parameters   Voltage between electrodes (ΔV)
                                                            Electrolyte properties
                             Electrolyte Temperature & pH




                 Temperature &
                  pH sensors                                       DAQ software




                                  Parameters
                              measurement system



S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress



        Electroforming process parameter tuning
        Electroformed copper parts with complex geometry
        Monitorization of parameters during the electroforming process
        Radiopurity measurements of electroformed copper parts
        Chemical & electrolytic improvements
        Electroforming in steps to fabricate cryostat copper components




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Review of objectives and work progress
  Preliminary radiopurity measurement of electroformed copper
 The levels of radiopurity in an electroformed copper part were previously measured
 with a HPGe detector (1Kg Ge) at the Canfranc Underground Laboratory (LSC).
                                                                         Radionuclide      Units (mBq/kg)
                                                            Th series        212
                                                                                   Pb              ≤ 16
        A standard- electroformed copper part
        (commercial chemicals & at sea level)                                228
                                                                                   Ac              ≤ 25
                                                            U series         234
                                                                                   Th              ≤ 32
                      Copper mass: 161 g
                                                                             234
                                                                                   Pa              ≤ 90
                      Measuring time: 5 d
                                                                                                   ≤e
                                                                                                      ss
                                                                             226
                                                                                   Ra              gr24
                                                                                             pro
                                                                                        t in        ≤3
                                                                             214
                                                                                   Pb
                                                                             214 m
                                                                                   en
                                                                             ure
                                                                                Bi                  ≤6

                                                                        m eas 235U                 ≤ 1.4
                                                                    w
                                                               Ne            137
                                                                                   Cs               ≤7
                                                                              40
                                                                                   K               ≤ 90
                                                                              60
                                                                                   Co               ≤7
     Copper part into a                 Copper around the                     56
                                                                                   Co               ≤3
     Marinelli container                 HPGe detector                        57
                                                                                   Co               ≤8
S. Borjabad 7th JRA-1 Zaragoza Nov´07                             (Data Analysis courtesy J. Puimedon)
                                                                             58                    ≤5
                                                                                Co
Review of objectives and work progress



          Electroforming process parameter tuning
          Electroformed copper parts with complex geometry
          Monitorization of parameters during the electroforming process
         ess
     rogrRadiopurity           measurements of electroformed copper parts
In p

          Chemical & electrolytic improvements
           eps
N   ext st
          Electroforming in steps to fabricate cryostat copper components




S. Borjabad 7th JRA-1 Zaragoza Nov´07
Summary and Prospects

     SUMMARY
   Electroformed copper parts with smooth surface and without machining
    can be manufactured by means of the tuning of process parameters.
   Copper parts with different geometry (hexagonal, cylindrical) can be
    achieved by easy modifications.
   Radiopurity measurements of electroformed copper parts are in progress.
   Soldering tests to join copper parts with electroformed copper are in
    progress.

     PROSPECTS
   Chemical & electrolitic improvements: CuSO4 purified by recrystallization,
    high- purity acids and anodes, CoSO4 and BaSO4 to reduce Co and Ra
    isotopes.
   Electroforming in steps to fabricate different copper parts such as cryostat
    components.
   This facility will be installed at the new (enlarged) Canfranc Underground
    Laboratory as soon as the clean room is ready.
S. Borjabad 7th JRA-1 Zaragoza Nov´07

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Copper Electroforming Process Monitoring and Optimization

  • 1. Copper Electroforming Status Report Silvia Borjabad 7th JRA-1 Meeting Zaragoza (November 2007)
  • 2. OUTLINE  Copper Electroforming Process  Review of objectives and work progress  Summary and prospects S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 3. Copper Electroforming Process Electroforming is a method of producing pieces by the deposition of a metal onto a mold (mandrel) which is subsequently removed Copper Electroforming Overview ENGINE • High-purity copper parts TANK • Accurate surface FILTER reproduction • Underground process • Chemical & electrolitic improvements CuSO 4 PUMP H 2SO4 S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 4. Copper Electroforming Process Process Parameters & Key Elements • Mandrel turns during the whole process producing a homogeneous deposition Constituents of the Electrolyte • Electrolyte circulates with continuous Constituent Concentration filtration to eliminate impurities • Covered bath avoids air and dust CuSO4 . 5H2O 188 g/l contamination H2SO4 75 g/l • Plating is done over polished and cleaned HCl 30 mg/l stainless steel mandrels with the same Thiourea 3 mg/l shape of the relevant copper parts (Brodzinski et al.,A292 (1990) 337) • H2SO4 improves the electric conductivity • HCl and Thiourea affect copper crystal nucleation and grain size S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 5. Copper Electroforming Process Electroforming Set-Up Voltage Supply Electronic Control System • Rotation Speed & Direction Electrolitic Bath • Plating modes • Electrolyte circulation • Inert cover gas (N2) Temperature and pH sensors • Temperature & pH sensors • Parameters DAQ system Filter and Pump S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 6. Review of objectives and work progress  Electroforming process parameter tuning  Electroformed copper parts with complex geometry  Monitorization of parameters during the electroforming process  Radiopurity measurements of electroformed copper parts  Chemical & electrolytic improvements  Electroforming in steps to fabricate cryostat copper components S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 7. Review of objectives and work progress Electroforming Process Parameter Tuning Smooth surface Goals Homogeneous copper distribution Without periodic machining process Parameters: Current Density, Speed Rotation and Direction Rotation Optimum parameters: 3 A/dm2, 2 rev/s, forward-reverse rotation S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 8. Review of objectives and work progress Electroformed copper parts with complex geometry • Hexagonal & cylindrical electroformed copper parts • Smooth Isolated areas surface with Teflon, parafine or • Accurate silicone surface reproduction (corners) 1.5 mm of thickness • Electroformed copper part for PMT encapsulation (collaboration ANAIS) • Smooth surface Isolated h wit gress • Homogeneous areas with s o est distribution Teflon t rp e ing g in Final machining r in • old rm S fo process r o Complex mandrel Auxiliary el ect 1.5-2 mm of thickness anode S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 9. Review of objectives and work progress  Electroforming process parameter tuning  Electroformed copper parts with complex geometry  Monitorization of parameters during the electroforming process  Radiopurity measurements of electroformed copper parts  Chemical & electrolytic improvements  Electroforming in steps to fabricate cryostat copper components S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 10. Review of objectives and work progress Parameters monitorization during the electroforming Current (I) Electroforming Evolution during the process Parameters Voltage between electrodes (ΔV) Electrolyte properties Electrolyte Temperature & pH Temperature & pH sensors DAQ software Parameters measurement system S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 11. Review of objectives and work progress  Electroforming process parameter tuning  Electroformed copper parts with complex geometry  Monitorization of parameters during the electroforming process  Radiopurity measurements of electroformed copper parts  Chemical & electrolytic improvements  Electroforming in steps to fabricate cryostat copper components S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 12. Review of objectives and work progress Preliminary radiopurity measurement of electroformed copper The levels of radiopurity in an electroformed copper part were previously measured with a HPGe detector (1Kg Ge) at the Canfranc Underground Laboratory (LSC). Radionuclide Units (mBq/kg) Th series 212 Pb ≤ 16 A standard- electroformed copper part (commercial chemicals & at sea level) 228 Ac ≤ 25 U series 234 Th ≤ 32 Copper mass: 161 g 234 Pa ≤ 90 Measuring time: 5 d ≤e ss 226 Ra gr24 pro t in ≤3 214 Pb 214 m en ure Bi ≤6 m eas 235U ≤ 1.4 w Ne 137 Cs ≤7 40 K ≤ 90 60 Co ≤7 Copper part into a Copper around the 56 Co ≤3 Marinelli container HPGe detector 57 Co ≤8 S. Borjabad 7th JRA-1 Zaragoza Nov´07 (Data Analysis courtesy J. Puimedon) 58 ≤5 Co
  • 13. Review of objectives and work progress  Electroforming process parameter tuning  Electroformed copper parts with complex geometry  Monitorization of parameters during the electroforming process ess rogrRadiopurity measurements of electroformed copper parts In p  Chemical & electrolytic improvements eps N ext st  Electroforming in steps to fabricate cryostat copper components S. Borjabad 7th JRA-1 Zaragoza Nov´07
  • 14. Summary and Prospects SUMMARY  Electroformed copper parts with smooth surface and without machining can be manufactured by means of the tuning of process parameters.  Copper parts with different geometry (hexagonal, cylindrical) can be achieved by easy modifications.  Radiopurity measurements of electroformed copper parts are in progress.  Soldering tests to join copper parts with electroformed copper are in progress. PROSPECTS  Chemical & electrolitic improvements: CuSO4 purified by recrystallization, high- purity acids and anodes, CoSO4 and BaSO4 to reduce Co and Ra isotopes.  Electroforming in steps to fabricate different copper parts such as cryostat components.  This facility will be installed at the new (enlarged) Canfranc Underground Laboratory as soon as the clean room is ready. S. Borjabad 7th JRA-1 Zaragoza Nov´07