Polymers under ionizing radiations : the specificity of Swift Heavy Ions

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1 Polymers under ionizing radiations : the specificity of Swift Heavy Ions Yvette Ngono-Ravache 1 (ngono@ganil.fr) M. Ferry 2, S. Esnouf 2, E. Balanzat 1 * 1 CIMAP, UMR CEA-CNRS-ENSICAEN-UCBN, BP 5133, F Caen cedex 5, France 2 CEA, DEN, DPC, SECR, LRMO, F Gif-sur-Yvette, France.

2 Polymers under Swift Heavy Ions (SHI) OUTLINE Introduction What is a polymer? Why is it necessary to study polymers under SHI? The specificity of SHI vs g and b Energy deposition pattern Dose distribution Some results and applications Influence of LET on defects creation How are SHI used to simulate a particles Conclusion date réunion

3 What are polymers? Polymers = long chains of atoms linked covalently and formed from a repeating unit (the moer in the case of homopolymers). Atoms currently present in repeating units : C, H, O, N, S Polymers are multi-scales materials Molecular scale: moer Macromolecular scale: chain Defect creation at the molecular scale = potential modifications on higher scales Supramacromolecular scale: chain network (physical or chemical links) Polymers are permeable to gases Polymers can be either amorphous or semi-crystalline Behavior under ionizing radiations function of the environment Gas emission possible under irradiation Behavior under storage function of the environment Study of polymer behavior under Ionizing Radiations very complex

4 Polymers under ionizing radiations Polymers are sensitive to ionizing radiations Bonds energy << energy deposited by ionizing radiations I.R Polymer Interactions with the electrons of the polymer Ionisations (x, PH +*, e - ) Excitations (PH*) Bond scission + reorganization Recombination h + -e - P + H Radical formation Radicalar chemistry Stable defects Macromolecular defects Gas emission

5 Radiation-induced defects under vacuum Macromolecular defects Polyethylene Unsaturated bonds New groups Chain scissions // Crosslinking H Gas emission (H 2, HCl, C x H y ) Cross-linking Vs Chain scissions Chain scissions in presence of Quaternary carbons (R 1 R 2 CR 3 R 4 ; R i H) Esters linkages (R 1 C(O)OR 2 ) H-transfer Degradation (chain scission) + Cross-linking preponderant in polymers with : -CH 2 CH 2 - suites -CH 2 -R 1 CH- suites Alkene groups Ulanski 2009 Cross-linking 5

6 G(gas) (10-7 mol.j -1 ) Polymer structure effect Under vacuum and in presence of gamma rays and electron beams: gas emission is function of the polymer chemical structure R=H or CH 3 Poly(methacrylic acid) R =OH or CH 3 R =H or F Polyisobutylene Polypropylene Polyethylene Polybutadiene Polyisoprene H 2 HCl or HF CO or CO 2 Polyvinyl chloride Polyvinylidene fluoride Polypropylene oxide Poly(ethylene oxide) Polyoxymethylene Poly(vinyl acetate) Poly(acrylic acid) Poly(methyl acrylate) Poly(vinyl alcohol) Poly(methyl methacrylate) Polychloro Polyglycolide prene Polyacrylo Polystyrene nitrile

7 Irradiation in presence of oxygen Oxidation O 2 H-transfer O-O Main Macromolecular Defects Carbonyls : Ketones: R 1 R 2 C=O Carboxylic acids: R 1 C(O)OH Esters: R 1 C(O)OR 2 Alcohols: R 1 R 2 R 3 COH Cambon Stéphanie PhD Thesis, Université Blaise Pascal, Clermont-Ferrand, 2001 Chain scissions (increase compared to irradiation under vacuum)

8 Radiation-Induced defects in polymers Under gamma ray and electron beam irradiations Radiation-induced defects depend on : The polymer structure Chemical structure of the repetition unit Crystalline ratio Irradiation conditions Dose and dose rate Surrounding atmosphere (inert or oxidative) Irradiation temperature What happens under Swift Heavy Ions? Linear Energy Transfer (g-rays and electrons vs SHI)

9 Why study SHI effects on polymers? Two fields of interest Basic science : Study of mechanisms underlying polymer radiation-induced ageing by Tuning the heterogeneous energy deposition pattern Kinetics Time scale of defects formation. Technological issues : Mainly radioactive waste storage Actinide-contaminated nuclear waste handling

10 Polymers widely used in nuclear industry 11% 1.3% Polyurethane 18.1% 40.5% Chlorinated polymers Polyolefins Polyamides 2.4% 10.1% 0.3% 16.3% Cellulose Fluorinated polymers Ion-exchange resin Other polymers MOx handling Human protection Surface protection Liquid effluent storage Contamination by radionuclides a, b, g radiations Medium Activity Long Life waste

11 Medium Activity Long Life waste Intended to Deep Repository Deep repository = different phases Filling Emission of hazardous gases Inflammability, corrosion Post-closure Macromolecular defects Polymer leaching Radionuclides complexation Safe management = What is the fate of polymers in conditions of long time periods and high doses? Well-chosen conditions Effects of a particles simulated by SHI

12 SHI : Energy deposition pattern Ion beam characteristics : Energy deposited along the path in a reduced space High LET Ion track = core + penumbra Track: Heterogeneous Track core: more or less homogeneous Energy deposited through interactions between : the ions and target electrons the secondary electrons and the target electrons Velocity effect Gervais&Bouffard NIMB 88 (1994) Radial distribution of dose Radius when E Dr 0.5 when E SHI = 2 Parameters (LET + Dr 0.5 )

13 Aim Swift Heavy Ions = High ionization/excitation densities How does high ionization/excitation densities modify the polymers ageing? Objectives Influence of dose and LET under inert and oxidative environments on: Gas emission Creation of new chemical groups (carbonyl groups, trans-vinylenes, vinyls, vinylidenes) Specific defects

14 METHODOLOGY Ion beams of various energies Basic science Ion beams of specific characteristics Simulation of a radiolysis date réunion

15 LET (kev/µm) Ion beams to simulate α irradiations? How to simulate a radiolysis by SHI irradiation? Equivalent LET Equivalent Dr medium energy GANIL high energy 160 µm 10 2 a particle Ne 40 µm C 10 1 He Energy (MeV/A) 870 µm Ar 7830 µm Electronic interactions Gervais & Bouffard, Nucl. Instrum. Methods Phys. Res., Sect. B 88 (1994), 355

16 LET (kev/µm) Ion beams to simulate α irradiations? How to simulate a radiolysis by SHI irradiation? Equivalent LET Equivalent Dr medium energy GANIL high energy SHI irradiation Vs a radiolysis 160 µm 10 2 a particle Ne 40 µm C 10 1 He Energy (MeV/A) 870 µm Ar 7830 µm Equivalent LET and Dr 0.5 Higher ranges for SHI Homogeneous LET Homogeneous irradiation under large thicknesses Gervais & Bouffard, Nucl. Instrum. Methods Phys. Res., Sect. B 88 (1994), 355

17 Irradiation procedures Irradiation of thin films On-line analyses (specific devices) Macromolecular defects Infrared spectroscopy Gas emission or O 2 consumption Mass spectroscopy (RGA mode) Off-line analyses : Two-step protocol Pre-ageing Up to high doses Determination of gas yields Reduced dose Ultra high-resolution gas mass spectrometry

18 Gas concentration [mol.kg -1 ] Irradiation procedures On-line analyses or two-step protocol Advantages Instantaneous cumulated yields Limitation in secondary reactions G(X) = f(polymer ageing level) Experimental points Cumulated formation rate at 3.4 MGy Instantaneous formation rate at 3.4 MGy Radiation chemical yield extrapolated at zero dose Chemical yield (G) G = number of moles of defects created per unit energy deposited Unit: mol/j Dose (D) Energy deposited per unit mass 0.1 Unit: Gy (Gray, 1Gy = 1J/kg) Dose [MGy]

19 RESULTS & APPLICATIONS date réunion

20 Specificity of SHI on defects creation Two groups of defects created under SHI Defects common to other ionizing radiations Influence on the relative radiation chemical yields Defects Specific to SHI G(defects) when LET

21 Specificity of SHI : Gas emission Primary effect = C-H scission H 2 emission common in organic molecules -(CH 2 -CH 2 ) n - -(CH 2 -CH) n - CH 3 Polyethylene Polypropylene -(CH 2 -CH) n - Polystyrene n PMMA LET influence on G(H 2 ) depends on the polymer structure Chang & LaVerne, J. Polym. Sci.: Part A: Polym. Chem. 38 (2000),1656

22 Specificity of SHI : Gas emission LET Effect on H 2 emission Almost inexistent on saturated polyolefines (PE, PP) LET influence on G(H 2 ) depends on the polymer structure Existent in presence of unsaturated bonds or more generally in presence of energy sinks PS: existence of a LET Threshold Below the threshold G(H 2 ) PS < G(H 2 ) PE Above the threshold G(H 2 ) PS G(H 2 ) PE Benzene ring destruction with LET = Protection efficiency lost

23 Specificity of SHI : Gas emission G total 4 2 PE PP PB CH (de/dx) (MeV mg -1 cm 2 ) 2 CH e LET influence on hydrocarbon gases (C x H y ) Low LET Polymer chemical structure signature High LET Loss of the polymer chemical structure signature C 2 H 5 Low LET Side group departure G side V. Picq, J.M. Ramillon, E. Balanzat, NIMB 146 (1998) V. Picq & E. Balanzat, NIMB 151(1999) High LET Chain fragmentation Very efficient PP, PB G total mol/j! Highly unsaturated gases

24 Specificity of SHI : Macromolecular defects Under Inert environment Evolution of Vinyl groups R-CH 2 -CH=CH 2 Unsaturated Bonds : LET influence function of the defect type Vinyl groups Concentration with LET High ionization densities mandatory Groups other than Vinyl At low doses : no LET effect At high doses : Concentration at saturation with LET Ngono-Ravache et al., Polym. Deg. Stab. 111 (2015), 89

25 Specificity of SHI : Defects specific to SHI Under Inert environment Specific defects Triple bonds ( Alkyne, Cyanates ) Cumulated double bonds ( Allene, Isocyanates ) Energy deposition time scale crucial simultaneity of ionization events RC CH RCH=C=CHR Existence of a LET Threshold f(defects, polymer structure) in presence of unsaturated bonds LET< LET Threshold Creation after a dose threshold date réunion

26 Application of SHI in the nuclear industry context : influence of SHI under O 2 Gas emission Macromolecular defects G(H 2 ) and G(oxidized groups) = f( dose) Various LET Under O 2

27 C(mol/kg) Specificity of SHI: oxidation Same oxidized defects as under gamma rays but with lower yields G(-O 2 ) 11 MeV/A 13C 0.2 *G(-O 2 ) 1MeV b Almost no LET effect on carbonyl containing functions Creation of unsaturated bonds under SHI cm cm cm-1 Ketones R 1 R 2 C=O Acids Ketones accumulate more rapidly Ratio ketone/acids with D 0.6 R 1 C(=O)OH G (acids) + G(Esters) with D 0.4 Esters 0.2 R 1 C(=O)OR Dose(Gy) CH CH 2 CH 2 2 CH m CH n CH2 EPDM 1,4 hexadiene CH 3 CH 2 CH CH p CH 3

28 C(mol/kg) Specificity of SHI : oxidation Almost no LET effect on any of the carbonyl containing functions cm cm cm-1 Ketones CH CH 2 CH 2 2 CH m CH n CH2 CH 3 CH 2 CH CH p CH R 1 R 2 C=O Acids EPDMn g rays (D< 500 kgy)* 0.6 R 1 C(=O)OH G(ketone)/G(acids) Esters Ion beam ( D<1500 kgy) G(ketone)/G(acids) = 4-5 R 1 C(=O)OR Dose(Gy) Ngono-Ravache et al., Polym. Deg. Stab. 111 (2015), 89 * Rivaton et al NIMB 227 (2005)

29 C(mol/kg) Specificity of SHI : oxidation Almost no LET effect on any of the carbonyl containing functions cm cm cm-1 Ketones R 1 R 2 C=O Acids CH CH 2 CH 2 2 CH m CH n CH2 CH 3 CH 2 CH CH EPDMn g rays (D< 500 kgy)* G(ketone)/G(acids) 3 p CH R 1 C(=O)OH Ion beam ( D<1500 kgy) 0.4 G(ketone)/G(acids) = 4-5 Esters 0.2 R 1 C(=O)OR Dose(Gy) (POOH ) II POO + POO P(O)OH HP P=O BMR

30 C(mol/kg) Specificity of SHI : oxidation Almost no LET effect on any of the carbonyl containing functions cm cm cm-1 Ketones R 1 R 2 C=O Acids CH CH 2 CH 2 2 CH m CH n CH2 CH 3 CH 2 CH CH EPDMn g rays (D< 500 kgy)* G(ketone)/G(acids) 3 p CH R 1 C(=O)OH Ion beam ( D<1500 kgy) 0.4 G(ketone)/G(acids) = Esters (POOH ) II P(O)OH HP R 1 C(=O)OR Dose(Gy) POO + POO P=O BMR Ratio BMR/HP when LET

31 C(mol/kg) Specificity of SHI : oxidation Unsaturated bonds : vinyl -HC=CH 2 Unsaturated bonds created under SHI but not under gamma LET1 LET2 LET3 Low Doses G 0 when LET 0.25 High doses Creation preponderant at high LET Onset of destruction at the lowest LET Dose(Gy) Same trend for vinylidenes and alkynes

32 Conclusion Basic research : modifying the heterogeneity of energy deposition gives insight on defects creation mechanisms. LET Effect on C=C Under vacuum on vinyl and defects specific to SHI Under oxidative environment On all defects Creation time scale < oxidation time scale LET effect on gas H 2 : Tremendous in presence of sinks after a threshold Hydrocarbon gases : tremendous date réunion

33 Conclusion Simulation of high dose deposition over long time periods Technological issues : Simulation of a particles with SHI Evolution of gas emission and carbonyls with the dose H 2 emission Oxidized defects Almost no effect on carbonyls but important dose effect in acids and esters with dose potential increase in hydrosoluble molecules Presence of C=C : great acceleration of oxidation at high doses date réunion

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