Présentation PowerPoint - 24th ICNTS

Présentation PowerPoint - 24th ICNTS

24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Christelle Bergeon 1, Christophe Mavon 1, Franck Berger 1, Zohra Lounis-Mokrani 2, Patrick Delobelle 3, Michel Fromm 1 1 : Laboratoire de Chimie-Physique et Rayonnement - Alain Chambaudet (LCPR-AC) UMR CEA E4, Universit de Franche-Comt. 16 route de Gray. F-25030 Besanon Cedex 2 : Laboratoire de Dosimtrie, Centre de Recherche Nuclaire dAlger, BP 399, Alger Gare 16000, Algeria 3 : FEMTO ST-LMARC. UMR 6174. 24, chemin de lpitaphe. 25030 Besanon cedex France. This paper mainly deals with changes in surface properties of an industrial polymer due to irradiations with gamma photons, electrons and alpha particles. In the second part of the presentation a discussion is presented that aims at comparing the dose (electrons, photons) effects with the fluence (alphas) effects, based on simple track structure theory. Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE The Polymer Under Study : PP / EPR / HDPE Plastics have become an important material for industrial applications, particularly in the automobile sector. Nowadays, plastics make up on average more than 15% of a vehicles weight. Polypropylene is the most commonly used polymer base. This material is the object of this study. Plastic parts are usually coated with paint and/or varnish. Workers in the industry have been trying to improve the coatings adherence properties for years. They often try to improve adherence by using a flaming treatment or a plasma technology. What are the effects of ionizing radiations on PP / EPR / HDPE surface and bulk properties ? Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE The Polymer Under Study : PP / EPR / HDPE is a ternary blend : isotactic polypropylene / ethylene-propylene rubber / high density polyethylene isotactic polypropylene polyethylene Scanning Electron Microscopy of the PP/EPR chemically etched in potassium permanganate in an acid medium

Radiation Induced Damage Brandon JP, Ph-D Thesis, University of Besanon, N 245, 1991. 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Irradiations Electrons: 10 to 106 Gy, 2 MeV, In air (Van de Graaf accelerator, Aerial, Strasbourg, France) Gammas: 10 to 106 Gy, 1.17 et 1.33 MeV, In air (60Co source, Alger, Algeria ) Alphas : 1011 to 1016 He+.cm-2, 400 keV, Under vacuum (Ion implantation, Lyon, France) The samples are exposed to electrons and gamma photons in air, as for the alpha particles, irradiation is performed under vacuum ! Radiation Quality Electron and gamma photon irradiations can be considered as uniform which is not the case for alpha particles (track structure and dependance on the fluence) The depth at which the incomming particles deposit their energy is very different as well as their stopping power : Radiation Induced Damage Oxygenation 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Analytical methods Irradiated samples have been analysed by means of: -FT-IR / ATR (Functional groups) -Contact angle (Surface energy, polarity, dispertion, ) - Nano-Indentation (Youngs modulus & Hardness) -Differential Scanning Calorimetry (Melting enthalpy & temperature) Swelling (Swelling ratio and soluble fraction) Radiation Induced Damage Surface properties Bulk properties 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Surface chemical modifications: FT-IR/ATR spectroscopy

CH3 H2 C C H2 C O2 H2 C CH3 H2 C C O O OH CH3 + + Gedde et al., J. Appl. Polym. 1990 5 2916 cm -1 1709 cm-1 : Carbonyl bond C O Gamma (9*10 Gy) Absorbance 2950 cm H2 C H2 C H -1 1375 cm-1

2871 cm-1 2839 cm-1 1456 cm O2 -1 0.05 Electrons (9*10 5 Gy) 1165 cm-1 3100 2700 2300 1900 Wavenumbers (cm -1 ) 1500 1100 Vacuum Spectrum of the pristine material + He (10 3100 2900 2700 2500 14 + -2 He .cm ) 2300 2100 1900

-1 1700 1500 1300 Wavenumbers (cm ) A. Chapiro, NIM B. 1988 H2 C H2 C Radiation Induced Damage -H2 H C H C H C H C 1630 cm-1 : vinylic function 1100 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results (alphas only) : Surface modifications: Contact angle Surface free energy versus fluence (m J.m -2) S 47 45 43 41 39 Untreted

Untreated 37 35 10 Radiation Induced Damage 11 12 13 + 14 -2 log(fluence (He .cm )) 15 There is a correlation between the increase in surface free energy and the loss of hydrogen (vinylic bond formation). 16 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Electrons and photons: Hardness & Youngs Modulus. Whatever electrons or photons were used the results obtained are similar when compared as a function of Dose Hardness and Young s modulus measured on the untreated and electron-irradiated (D = 910 5 Gy) smple s surfce . 100 H (MPa) 2.2 E (GPa) 90 2 80 1.8 70 910 5 G y 60

Untreated 910 5 G y 1.6 Untre te d 1.4 50 1.2 40 30 1 0 500 1000 1500 2000 h (nm) Radiation Induced Damage 2500 3000 3500 0 500 1000 1500 2000 h (nm) 2500 3000

3500 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Nano-indentation curves for alpha & electron irradiated samples. P (mN) 14 P (mN) 14 12 1016 He+ .cm-2 The visco-elastic behaviour does not remain after irradiation 10 9 10 5 G y 12 The visco-elastic behaviour remains 910 4 G y 10 Untreated 8 8 1015 He+ .cm-2 6 1014 He+ .cm-2 4 Untreated 2 6 4 2

0 0 0 500 1000 h (nm) 1500 2000 0 500 1000 1500 2000 2500 3000 h (nm) The material was more fragile after the ion treatment since the analyzed surface is a hard film (the irradiated part is 2.3 m) on a soft substrate (the untreated part). Alpha particles gradually lose their energy as they penetrate the PP/EPR up to about 2.3 m. For samples irradiated with electrons, H and E remain constant within the domain of the studied indentation depth. Indeed, in this case, we can consider that the electrons regularly lose their energy up to h = 3000 nm. Radiation Induced Damage 3500 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Swelling for gamma & electron -irradiated samples. In order to study the crosslinking of the PP /EPR, the samples were analyzed using the swelling technique. Swelling was performed in two different liquids. First, the studied samples were dipped into 1,2-dichorobenzene, a PP/EPR solvent, at 130C for about one hour. Thus, the crosslinking network, insoluble in the solvent, could be studied. Some samples were also dipped into hexane in order to obtain information about the PP/EPR samples that were either untreated or irradiated at weak doses and fluences. This liquid is not a PP/EPR solvent but it has a good affinity with him.

Immersion in 1,2 -dichlorobenzene after irradiation at an electron dose of 9 . 105 Gy. We observe the crosslinking effect. Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 m m 21 t= m 1 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Swelling in hexane for gamma & electron -irradiated samples. t 0.23 0.22 Un tre te d 0.21 m1 is the samples mass after one day of swelling and hexane evaporation; and m2 is the samples mass after a second swelling in hexane during a period of 46 days. 0.2 0.19 0.18 Ele ctron G m m 0.17 0.16 0.15 0 1 2 3

4 log(Dose (Gy)) provides information on the crosslinking part of the sample. Radiation Induced Damage 5 6 7 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Differential Scanning Calorimetry Thermogramms of untreated and -irradiated PP/EPR 0 m W / m g --0 ,0,2 P E H D 4 --0 ,0,6 P P E n d o 8 --1,1 5G 2 9 . 4 1 0 y 5G --1 ,1,4

4 1 0 y 6 G y180 -1,880 10 120 140 1600 T em perature(C ) Melting peaks for the two main components of the compound, i.e. PP and HDPE Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Results : Differential Scanning Calorimetry 170 1 65 T melting PP (C) Untreated 165 T m e lting P P (C) Untre ate d 1 64 1 63 160 1 62 155 Electron Gamma 150 1 61 1 60 145

1 59 1 58 140 0 1 2 3 4 5 6 13 7 13 .5 H 80 -1 m e ltin H 75 PP (J. ) 75 14 14 .5 15 15 .5 log (flue n ce (He +.c m -2 )) log(Dose (Gy)) m e ltin PP (J.-1 ) Un tre te d

65 Un tre te d 70 55 65 45 Ele ctron G m m 60 35 25 55 15 50 0 1 2 Radiation Induced Damage 3 4 log(Do s e (G y)) 5 6 7 13 1 3.5 14 14 .5 + 15 -2

lo(flue nce (He .cm )) 15 .5 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Comparison : Critical doses and fluences where the studied properties are greatly modified ( : electrons, : gamma photons, p : alphaparticles). 0 Y o u n g 's m o d u lu s Y o u n g 's m o d u lu s H a rd n e s s H a rd n e s s S w e llin g S w e llin g M e lt in g t e m p e r a t u r e M e lt in g t e m p e r a t u r e F T -IR /A T R F T - IR / A T R 1 2 3 4 lo g ( D o s e ( G y ) ) Radiation Induced Damage 5 6 7 10 11 12

13 14 lo g ( F lu e n c e ( H e 15 + .c m -2 16 )) 17 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Dose & Fluence : The changes in the compound properties were observed from a critical dose ( 105 Gy) or critic l fluenc e (510 13 He +.cm -2 ). For the ion irradiation, the track overlapping can explain most of the observed effects: 10 11 i ons. c m -2 10 12 i ons. c m -2 10 13 i ons.

c m -2 scale: 20 nm/division See the work by Yamauchi But, is there a way to transform a dose into a fluence or reciprocally ? Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Dose - Fluence Relation ? E Rr LET r Equivalent Dose Calculation for f = 5 .1013 He+.cm-2 In Polyethylene D= 1000 300 TEL(keV.m-1) 250 200 150 100 50 0 0 100 200 Radiation Induced Damage With electrons and gammas in air, we find LET = 199 keV.m-1, or 1.99106 keV.c m-1 300 Energy(keV) D=

-1 1.5107 J.k 400 -1 1.8107 J.k D = 105 Gy 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Dose - Fluence Relation ? Deposited dose by an helium ion (400 keV) in the polypropylene versus the distance to the track center r and versus the particle energy E. The latent track rt 0 1 10 102 103 104 C 20 o re halo R 40 t r 60 a c 80 k 100 x(m) r(nm) (a) (b) Do6se ( 10 Gy) 4 3 2 1 0 5 r(nm) 10 400 3 0 0

2 0 0 15 0 100 E(keV) Matlab calculation based on: Vareille, J.C. PhD Thesis, University of Limoges, Limoges, France, 1982. Radiation Induced Damage Waligorski, M.P.R. ; Hamm, R.N.; Katz, R. Nucl Tracks Radiat Meas 1986, 11(6), 309-319. 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Dose - Fluence Relation ? f = 5 .1013 He+.cm-2 Dose inside the latent track ) 110 Depositedtotaldose(% 100 90 80 70 60 50 40 30 0 1 2 3 4r(nm 5) 6 7 8 9 Covered surface fraction 1 0.8 0.6 r = 5 nm 0.4 0.2 0 9 10 11 12 13 + 14 15

-2 log(fluence (He .cm )) With the MATLAB software, the deposited total dose along the ions range can be estimated: D 310 7 Gy. To be compared with Radiation Induced Damage D = 105 Gy ! 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Conclusions Creation of carbonyl bonds in the case of a treatment under air (electrons and ) and the formation of vinylic groups after irradiation with ions under vacuum For similar doses, the studied effects are equivalent after electron or irradiation. For the three kind of irradiation used (electrons, , He+), the studied properties are notably modified for fluences above 510 13 He +.cm -2 in the cse of lph prticl e s nd for dose s in 5 6 the order of 10 - 10 G y in the cse of electronsnd m m photons. The difference in the irradiation atmosphere (vacuum for alpha particles and air for electro ns and ) and in the nature of th e transformations induced by radiations (high LET for alpha particles and low LET for el ectrons and ) seem to b e responsible for the observed differences. Radiation Induced Damage 24th ICNTS, Bologna, 1-5 September 2008 Electron, Gamma Photon and Ion Irradiation Effects in PP/EPR/HDPE Radiation Induced Damage

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