CHANDA workshop on target preparation – the needs and the ......CHANDA workshop on target preparation – the needs and the possibilities Goedele Sibbens E-mail: [email protected]

CHANDA workshop on target preparation –the needs and the possibilities

Goedele Sibbens

E-mail: [email protected]

Paul Scherrer Institute, Villigen

23-25 November 2015

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Target preparation and characterization at JRC-IRMM

Goedele Sibbens, André Moens, David Vanleeuw, David Lewis, Ananda Sagari Arcot Rajashekar,

Yetunde Aregbe

Goedele SibbensResponsible Target Preparation [email protected]

PSI VilligenCHANDA workshop

on target preparation23-25 November 2015

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Target preparation techniques

� Molecular plating

� Vacuum deposition

� Mechanical techniques

� In-situ polymerization

Target characterization techniques

� Weighing

� Alpha-particle counting at a defined solid angle

� Combustion analysis

� Spectrophotometry

This presentation



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Molecular plating



The method is based on the cathodic deposition

of the material onto a backing from isopropanol.

Polyacetal

Cathode

Rotating Pt anode

Stainless Steel

Stainless Steel backing holder and sealing ring

Molecular plating cell

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238U layer

material: 99.999% 238U

method: molecular plating

deposit diameter: 30 mm

backing: 0.25 mm Al Ø 50 mm

mass 238U: 1.9 mg

areal density 238U: 265 µg.cm-2

TP2010-011-07

TP2015-007-05

U thin layer target



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237Np layer

material: 237Np




Mass 237Np: 1.4 mg

areal density 237Np: 204 µg.cm-2

TP2010-011-07

TP2014-010-09

Np thin layer target



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235U layer

material: 99.934% 235U




Mass 235U : 3.5 mg

areal density 235U: 279µg.cm-2

TP2010-011-07

TP2015-008-03

U thin layer target



Molecular plating

To produce thin layers of

U, Pu, Np, Am isotopes

Ø layer 5-60 mm

Areal density: 10-300 µg/cm2

Backing: Al Ø 10-80 mm

� G. Sibbens, A. Moens, R. Eykens, D. Vanleeuw, F. Kehoe, H. Kühn, R.

Jakopic, S. Richter, A. Plompen, Y. Aregbe, Preparation of 240Pu and 242Pu

targets to improve cross section measurements for advanced

reactors and fuel cycles, J Radioanal Nucl Chem (2014) 299:1093–1098

� L. Benedik, G. Sibbens, A. Moens, R. Eykens, M. Nečemer, S. D. Skapin, P.

Kump, Preparation of thick uranium layers on aluminium and

stainless steel backings, Appl Rad Isot (2014) 87:238-241



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Heated coating material in Ta crucible

Vacuum

Vapour

Deposit

Backing mounted on a rotating carrousel

Backing

Backing holder

Mask

Thickness monitor

The method is based on the condensation

of a vaporized substance onto a backing


on target preparation23-25 November 2015Vacuum deposition

Vacuum deposition

connection to electrodes

Ta crucible with 235UF4

diaphragm

carrouselquartz crystal

shutter

mask

backing with 235UF4 deposit

glass bell jar with metal cage

235UF4 evaporator



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material: 235UF4

method: vacuum deposition


backing: 0.25 mm Al Ø 72.9 mm

mass 235U : 6.2 mg

areal density 235U : 318 µg cm-2

TP-NP 08-65-02

U thin layer target



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238UF4 evaporator (new)

Vacuum deposition



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material: 238UF4




mass 238U : 0.8 mg

areal density 238U : 114 µg cm-2

TP2010-011-07

TP2015-014-12

U thin layer target



material: 238UF4



backing: 0.25 mm StSt Ø 50 mm

mass 238U : 0.3 mg

areal density 238U : 48 µg cm-2TP2015-014-15

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� 6LiF heated in Ta crucible to 845ºC

� depos. rate 0.05 - 0.4 nm/s

� metallicLi heated in Alumina crucible

in Ta crucible heater to 600ºC

� depos. rate about 0.35 nm/s

� Au layer to provide electric conductivity

� Au heated in Ta crucible to 1064ºC

� deposition rate 0.01 - 0.05 nm/s



Au evaporator

Li evaporator

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Lithium -gold layer

material: 6LiF and Au


backing: 41 µg cm-2 PI foil Ø 50 mm

deposit diameter Au: 48.9 mm

mass Au: 0.8 mg

areal density Au: 43 µg cm-2

deposit diameter 6LiF: 30 mm

mass 6LiF: 0.1 mg

areal density 6LiF: 14 µg cm-2

TP2010-011-07

TP2015-012-02

Li-Au thin layer target



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� C57H110O6 heated in Ta crucible to 60ºC

� deposition rate 0.1 - 1.5 nm/s



Tristearin evaporator

new evaporatorhome-made

in construction phase

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tristearin layer

material: C57H110O6



backing: 0.1 mm Ta Ø 35 mm

mass C57H110O6 : 36 mg

areal density C57H110O6 : 7213 µg cm-2

TP2010-011-07

TP-NP 07-26-07

Tristearin target



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10B evaporator

� 10B heated by bent electron

beam in Cu crucible to 2076ºC

� depos. rate 0.02 - 0.05 nm/s

Vacuum deposition



Vacuum deposition

To produce thin layers of 235U and 238U

Ø layer 5-60 mm


Backing: Al, StS, PI foil Ø 10-80 mm

� G. Sibbens, A. Moens, D. Vanleeuw, R. Eykens, S. Oberstedt, Multi-

layer 235UF4-6LiF-Au targets for high-resolution fission fragment

measurements, Appl Rad Isot (2014) 87:229-232

� G. Sibbens, A. Moens, R. Eykens, Preparation and sublimation of

uranium tetrafluoride for the production of thin 235UF4 targets, J

Radioanal Nucl Chem (2015) 305:723-726



Vacuum deposition

To produce thin layers of 6LiF, natLiF, 7LiF, metLi, Au, C57H110O6 and 10B

Ø layer 5-80 mm


Backing: Al, Ag, Au, StS, Si, Ta, PI foil Ø 10-130 mm

� D. Sapundjiev, A. Dean, U. Jacobsson, K. Luyckx, A. Moens, G. Sibbens,

R. Eykens, Y. Aregbe, Preparation and characterisation of thin film

nuclear targets for neutron physical measurements, Nucl Instr

Meth A 686 (2012) 75–81

� D. Vanleeuw, D. Sapundjiev, G. Sibbens, S. Oberstedt, P. S. Castiñeira,

Physical vapour deposition of metallic lithium, J Radioanal Nucl

Chem (2014) 299:1113–1120



Mechanical techniques

Rolling foilsmaterial: Al, other metalsthickness 1.0 – 0.05 mm

Drawing wiresmaterial: Al alloysØ 1.0 – 0.5 mm

Punching discsmaterial: metals, thickness < 0.3 mmØ 1 – 100 mm

Pressing powdersTotal mass by weighing: readability 10 µg



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Punching discs of metals

with thickness < 0.3 mm and diameter 1-100 mm

Drawing wires of Al alloys

with diameter 1.0-0.5 mm


on target preparation23-25 November 2015Mechanical techniques

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Preparation of alloys by arc-melting

Rolling foils of Al or other metalswith thickness 1.0-0.05 mm




Pb -7.5% In

Na disc prepared by cutting, pressing, mechanical rolling and punching

Pressing of powder compacts




Hydraulic press in glove boxHydraulic press

S pellet Ø30mmPress force 200kN

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Preparation of powder pellets with an hydraulic press

Fume dust pelletin an Al cup




Pressing of powder compacts

positioning of the Al cup in the matrix


Canning powder in Al container



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Polymerization

Preparation of polycondensate solution1,2,4,5 - benzenetetracarboxylicdianhydrid + 4,4‘ – diaminodiphenyletherin N,N' – dimethylformamide(dry atmosphere!)

Polymerization 12 min at 350ºC

covering the glassplates with polycondensatesolution

transfer of polyimide foil onto ring



To produce thin polyimide foils

Ø 10-90 mm


�mechanically strong

�excellent resistance to

- irradiation with charged particles

- temperature

- chemicals

�not commercially available at thickness of interest

� G. Sibbens, K. Luyckx, A. Stolarz, M. Jaskóła, A. Korman, A. Moens, R.

Eykens, D. Sapundjiev, Y. Aregbe, Quality of polyimide foils for

nuclear applications in relation to a new preparation procedure,

Nucl Instr and Methods in Physics Research A 655 (2011) 47–52



Polymerization

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Thickness, diameter and mass determination

Characterisation



Microbalancemax 52 g d=0.001 mg

� Thickness and diametercaliper: readability 10 µmmicrometer: readability 1 µm

� Massweighing: readability 1 µg

At IRMM

� Thermal ionization mass spectrometry

(actinides)

� Atomic force microscopy (stable)

� Scanning electron microscopy (stable)

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Activity measurement by low-geometry alpha-particle counting

LG2LG3

Detector

diaphragm

Ø 20mm

Actinide target

50 200 mm

Detector

diaphragm

Ø 17mm

Actinide target

16

37

mm

LG2


on target preparation23-25 November 2015Characterisation

Homogeneity measurement of thin actinide layers

by low-geometry alpha-particle counting

Characterisation



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reflection mode

transmission mode

Characterisation

Thickness measurement of

polyimide foils by

photospectrometry



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Combustion analysis

with CHN analyser (Elementar Vario EL III)

� Sample weighing and calibration

� Percentage of element content of C, H and N

Oxidation: C,H,N

Reduction: NO x �N2

Adsorption

Measurement:

N2, H2O and CO2

Characterisation



Characterisation

� Weighing

� Alpha-particle counting at a defined solid angle

� Combustion analysis

� Spectrophotometry

� J. Heyse , M. Anastasiou , R. Eykens, A. Moens, A. Plompen, P. Schillebeeckx, G.

Sibbens, D. Vanleeuw, R. Wynants, Characterization of 235U targets for the

development of a secondary neutron fluence standard, J Radioanal Nucl Chem

(2014) 299:1055–1059

� D. Sapundjiev, A. Dean, U. Jacobsson, K. Luyckx, A. Moens, G. Sibbens, R. Eykens, Y.

Aregbe, Preparation and characterisation of thin film nuclear targets for neutron

physical measurements, Nucl Instr Meth A 686 (2012) 75–81

� D. Vanleeuw, G. Sibbens, A. Plompen, Determination of the hydrogen content of

thick tristearin layers prepared by physical vapour deposition, J Radioanal Nucl

Chem (2015) 305:957-962



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Customers

� IRMM GELINA and Van de Graaff accelerator

� CHANDA

� EUFRAT



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Thank you for your attention !



Goedele SibbensResponsible Target Preparation [email protected]

Documents

CHANDA workshop on target preparation – the needs and the ......CHANDA workshop on target preparation – the needs and the possibilities Goedele Sibbens E-mail: [email protected]