Quality of polyimide foils for nuclear physics applications in - - PowerPoint PPT Presentation

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VANCOUVER 12-17 September 2010 INTDS 2010 1 Quality of polyimide foils for nuclear physics applications in relation to a new preparation procedure G. Sibbens, K. Luyckx, A. Stolarz, M. Jask a, A. Korman A. Moens, R. Eykens, D.

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SLIDE 1

IRMM - Institute for Reference Materials and Measurements Geel - Belgium http://irmm.jrc.ec.europa.eu/ http://www.jrc.ec.europa.eu/

Quality of polyimide foils for nuclear physics applications in relation to a new preparation procedure

  • G. Sibbens, K. Luyckx, A. Stolarz, M. Jaskóła, A. Korman
  • A. Moens, R. Eykens, D. Sapundjiev, Y. Aregbe

VANCOUVER 12-17 September 2010 – INTDS 2010 1

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VANCOUVER 12-17 September 2010 – INTDS 2010 2

IRMM and Target Preparation Laboratory Purpose of the work Method to prepare polyimide foils Standard procedure and modifications Mechanical, heat and irradiation tests Impurities Conclusion

This presentation

Quality of polyimide foils for nuclear physics applications in relation to a new preparation procedure

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VANCOUVER 12-17 September 2010 – INTDS 2010 3

Institute for Reference Materials and Measurements

Analytical laboratories Radionuclide metrology laboratories Underground laboratory Two accelerators for neutron production

150 MeV linear electron accelerator (GELINA) 7 MV light-ion Van de Graaff accelerator

Reference materials production and storage

http://irmm.jrc.ec.europa.eu/ http://www.jrc.ec.europa.eu/

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 4

Thin 235U targets by vacuum deposition

vacuum deposition of 235UF4 from a resistance-heated Ta-crucible source

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 5

Thin actinide targets by electrodeposition

electrodeposition of e.g. UO2(NO3)2

  • n metallic backing in isopropanol

233U, 235U, 240Pu, 242Pu

  • C. Ingelbrecht et al. Nucl. Instr. and Meth. in Phys. Res. A 397 (1997) 34-38

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 6

Characterisation of thin actinide targets

activity measurement and distribution of the active material by low-geometry alpha counting using a Si surface barrier detector.

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 7

Thin film nuclear targets

Thin deposits of :

  • 6LiF, nat. LiF
  • 10B
  • Au
  • tristearin

Characterisation:

  • Total mass of deposit by weighing
  • Amount of atoms (6Li, nat. Li,10B, H) by ?

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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SLIDE 8

VANCOUVER 12-17 September 2010 – INTDS 2010 8

Target preparation at IRMM

Mechanical transformation techniques:

  • Rolling

thin metallic foils: thickness 1.0 – 0.05 mm

  • Wire drawing

thin metallic wires: Ø 1.0 – 0.5 mm

  • Punching

metallic discs Ø 1 – 100 mm, thickness < 0.5 mm

  • Pressing

homogeneous powder compacts

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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SLIDE 9

VANCOUVER 12-17 September 2010 – INTDS 2010 9

Target preparation at IRMM

Polyimide foils

areal density 20 - 500 µg·cm-2

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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SLIDE 10

VANCOUVER 12-17 September 2010 – INTDS 2010 10

Purpose of the work

To investigate if polyimide foils

for nuclear physics applications with an areal density around 35 µg·cm-2 prepared in another and faster way than the standard procedure have similar or better properties

  • good resistance to temperature
  • good resistance to irradiation with charged particles
  • mechanically strong

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 11

Preparation method of polyimide foils

1979 Pauwels et al. developed method at IRMM via amide-acid spreading in situ polymerisation on glass plates

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 12

Preparation method for thin polyimide foils

1,2,4,5 - benzenetetracarboxylicdianhydrid + 4,4‘ - diaminodiphenylether N,N' – dimethylformamide

preparation of polycondensate solution

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 13

Preparation method for thin polyimide foils

cleaning the glassplates 4h at 100°C 12 min at 350°C covering the glassplates with the polycondensate solution

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 14

Preparation method for thin polyimide foils

transfer of polyimide foil onto frame

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 15

Characterisation of polyimide foils

thickness measurement with spectrophotometer reflection mode transmission mode

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 16

Preparation of polyimide foils at IRMM

1979 Pauwels et al. developed method at IRMM

via amide-acid spreading and in situ polymerisation on glass plates 4 hours at 100 ºC, 25 hours at 230 ºC

1981 Van Gestel et al.

4 hours at 100 ºC, 30 min at 340 ºC stronger foils

1995 Eykens et al.

dry atmosphere 4 hours at 100 ºC, 15 min at 360 ºC stronger foils

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 17

laminar flow laminar flow laminar flow laminar flow foil transfer

  • ven

12 min 350 °C

  • ven

12 min at 350 °C

  • ven

4 h at 100 °C 12 min at 350 °C

  • ven

4 h at 100 °C 12 min at 350 °C thermal treatment Ar-glove box fume hood Ar-glove box fume hood spin coating Ar-glove box fume hood Ar-glove box fume hood polycondensate Fast procedure in argon Fast procedure in air Standard procedure in argon Standard procedure in air Preparation step

Foil preparation procedures

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 18

Quality tests

Resistance to heat Pressure test Dropping test Irradiation with charged particles

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 19

Resistance to heat

20 min 360 ºC 20 min 380 ºC 20 min 400 ºC foils 34 µg·cm-2 standard in air fast in argon

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 20

Pressure test

foils 20 µg·cm-2 - 80 µg·cm-2 standard in air standard in argon fast in air fast in argon rupture coefficient R in J·kg-1 of Chen R = p * D / t p = pressure in Pa D = diameter foil in cm t = areal density foil in mg·cm-2

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 21

Dropping test

foils 20 µg·cm-2 - 30 µg·cm-2 standard in argon fast in argon foils 35 µg·cm-2 - 55 µg·cm-2 standard in air fast in argon

maximum 1.7 m

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 22

Irradiation

foils 40 µg·cm-2 - 47 µg·cm-2 standard in air standard in argon fast in air fast in argon

  • n frames with aperture Ø 15 mm

Van de Graaf accelerator of SINS in Warsaw 2.0 MeV single charged 4He ions 1.5 MeV protons beam spot of 4 mm

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 23

Areal density range µg·cm-2 20 - 30 35 - 55 35 - 55 70 - 80 Argon Air Argon Air Procedure Standard Fast Standard Fast Standard Fast Standard Tests Heat resistance temp [ºC] 380 400 380 Pressure R [J·mg-1] 0.25(5) 0.15-0.30 0.20(5) 0.17(6) 0.22-0.26 0.20-0.27 Dropping height [m] 0.9(3) 1.0(3) 3.7(5) 3.6(4) Irradiation 2.0 MeV 4He+1 beam intensity [nA] 500 500-900 800 500 deposited beam power [W] 3.3·10-2 (3.3-5.9)·10-2 5.3·10-2 (3.3-5.9)·10-2 charge [C] 3.0·10-4 (4.5·-15)·10-4 5·10-4 4.0·10-4 Irradiation 1.5 MeV protons beam intensity [nA] – – 400-4500 800 700-1000 800-1500 – deposited beam power [W] – – 3.3·10-3- 3.7·10-2 6.5·10-3 (5.7-8.15)·10-3 6.5·10-3-1.2 10-2 – charge [C] – – (0.3-2.1)·10-3 1.2·10-3 9·10-4-1.1·10-3 (0.6-1.1)·10-3 –

Summary

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VANCOUVER 12-17 September 2010 – INTDS 2010 24

Pressure test

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 10 20 30 40 50 60 70 80 foil thickness ug/cm2 rupture coefficient J/mg

standard in air standard in argon fast in air fast in argon

areal density

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 25

Strength for 20 µg·cm-2 foils

  • R. Eykens, P. Maier-Komor, J. Van Gestel. J. Pauwels, Nucl. Instr. and Meth. A 362 (1995) 175

fast argon

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 26

Areal density range µg·cm-2 20 - 30 35 - 55 35 - 55 70 - 80 Argon Air Argon Air Procedure Standard Fast Standard Fast Standard Fast Standard Tests Heat resistance temp [ºC] 380 400 380 Pressure R [J·mg-1] 0.25(5) 0.15-0.30 0.20(5) 0.17(6) 0.22-0.26 0.20-0.27 Dropping height [m] 0.9(3) 1.0(3) 3.7(5) 3.6(4) Irradiation 2.0 MeV 4He+1 beam intensity [nA] 500 500-900 800 500 deposited beam power [W] 3.3·10-2 (3.3-5.9)·10-2 5.3·10-2 (3.3-5.9)·10-2 charge [C] 3.0·10-4 (4.5·-15)·10-4 5·10-4 4.0·10-4 Irradiation 1.5 MeV protons beam intensity [nA] – – 400-4500 800 700-1000 800-1500 – deposited beam power [W] – – 3.3·10-3- 3.7·10-2 6.5·10-3 (5.7-8.15)·10-3 6.5·10-3-1.2 10-2 – charge [C] – – (0.3-2.1)·10-3 1.2·10-3 9·10-4-1.1·10-3 (0.6-1.1)·10-3 –

Summary

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VANCOUVER 12-17 September 2010 – INTDS 2010 27

Irradiation

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

resisted a beam up to 4.5 µA resisted a beam of only 50 nA

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VANCOUVER 12-17 September 2010 – INTDS 2010 28

200 400 600 800 1000 1200 1400 1600 1 2 3 3 4 5 5 6 7 8 energy [keV] counts

standard in air (foil #20) standard in air (foil #17) fast in air (foil #12) standard in argon (foil #15) fast in argon (foil #16)

Zn Si Al S Cl K Ca Cr Ti Fe Mn Cu

Impurities in the polyimide foil by PIXE

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 29

Impurities in foil and bulk material

element impurity in polyimide [mg·kg-1] PIXE - foil NAA - bulk Ca (0.40 - 0.90)·10-3 < 0.4·10-6 Cl (0.15 - 0.28)·10-3 1.9·10-6 Fe (0.15 - 0.98)·10-3 (8.3 ± 1.0)·10-6 K (0.20 - 0.94)·10-3 (0.62 ± 0.08)·10-6 Mn (0.03 - 0.30)·10-6 (0.068 ± 0.002)·10-9 S 0.21 - 0.42 < 20·10-3 Ti (0.02 - 0.29)·10-3 < 1.5·10-6

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 30

Conclusion

fast preparation way in a dry atmosphere improved mechanical and thermal strength life time under charged particles less impurities in the foil stronger foils new procedure:

fast preparation way in a dry atmosphere

intro --- purpose --- method --- modifications in procedure --- tests --- impurities --- conclusion

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VANCOUVER 12-17 September 2010 – INTDS 2010 31

Thank you for your attention !