Studies on Neon irradiated amorphous carbon using X-ray Diffraction. technique

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1 Studies on Neon irrdited morphous rbon using X-ry Diffrtion tehnique A.Srkr *, K. Dsgupt #, P. Brt P. Mukherjee *, D. Sthiymoorthy # * Vrible Energy Cylotron Centre, 1/AF Bidhn Ngr, Kolkt , Indi # Mterils Group, Bhbh Atomi Reserh Centre, Mumbi , Indi Abstrt Two sets of morphous rbon mterils prepred t different routes re irrdited with swift (145 MeV) hevy ion (Ne 6+ ). The struturl prmeters like the size of ordered grins long nd xis i.e. L & L, the verge sping of the rystllogrphi plnes (00) i.e. d 00 nd the frtion of the morphous phse of the unirrdited nd the irrdited smples re estimted by X-ry diffrtion tehnique. The frtion of the morphous phse is generlly found to inrese with the irrdition dose for both sets of the smples. The estimted d 00 nd L vlues re found to be lmost unffeted by irrdition. The estimted vlues of L orroborte with the inrese of disorder in both sets of the smples with the inresing dose of irrdition. Keywords: X-ry Diffrtion, Amorphous Crbon, Irrdition Introdution The effets of prtile irrdition in solids hve been field of intense reserh sine 1950s. The erly studies foused on rdition dmge in mterils of nuler tehnology to understnd the vrition of their physil nd mehnil properties due to irrdition. The llotropes of rbon hve been the subjet of mny erly studies; in prtiulr grphite hs ttrted muh ttention s nuler retor mteril in Corresponding uthor, Emil: pbrt@vel.ernet.in 1

2 retors. Moreover in reent yers the development of proper struturl mterils for fusion retors where rbon is onsidered to be one of the potentil ndidte mteril, is hllenging job to the nuler tehnologists. From the renewed interest in rdition dmge in rbon strutures need for the genertion of dt bout the behvior of rbon mterils under prtile irrdition hs risen. The use of grphite s modertor in high temperture nuler retors is well known [1]. However, in low temperture therml nuler retors, grphite nnot be used s modertor due to the possibility of sudden relese of the stored energy (Wigner energy) [1, ] in it, resulting from the displement of toms from its lttie position during irrdition. Clultion shows tht this stored energy my get relesed suddenly round 00 C nd n led to n ident in the therml nuler retors [1,]. Use of morphous rbon s modertor n eliminte the Wigner energy effet. To develop suh novel rboneous mteril to be used in the nuler retor, two sets of smples of morphous rbon hve been prepred following different routes. It is interesting to study whether the prtile irrdition uses formtion of ny rystlline phse in the morphous rbon smples. This study will help us to be sfe in using the morphous rbon smple s modertor in the low temperture therml nuler retors. During irrdition the inident prtiles deposit kineti energy in the lolized sptil region of the irrdited smples. There is possibility tht this deposited energy n use lolized ordered rrngement in the disordered struture of the toms in the morphous smples leding to rystllinity. In the present work, we hve rried out irrdition with 145 MeV Ne 6+ ions on the morphous rbon smples t different doses. We hve hrterized the struturl

3 prmeters like the size of the ordered grins long nd xis i.e. L & L, the verge sping of the rystllogrphi plnes (00) i.e. d 00 nd the frtion of morphous phse of the unirrdited nd the irrdited smples s funtion of dose using the X-ry diffrtion (XRD) tehnique. The dmge profile s funtion of depth from the surfe of these smples hs been hrterized in terms of displement per tom (dp) for different doses. Experimentl Smple preprtion: Two types of morphous rbon hve been prepred. Smple A ws prepred with 15% rbon blk dispersed in phenoli resin. The smple ws rbonized t C with heting rte of C /hr in rgon tmosphere. Smple B ws prepred from hopped PAN fiber in resin mtrix. The smple ws then rbonized t C in rgon tmosphere with heting rte of 60 0 C/hr. Irrdition experiment: The smples A nd B were mounted on n luminum flnge nd then irrdited with 145 MeV Ne 6+ ions from Vrible Energy Cylotron (VEC), Kolkt, Indi. The irrdition doses were , , Ne 6+ /m. The flnge used in irrdition ws ooled by ontinuous flow of wter. During irrdition, the temperture of the smples did not rise bove 313K s monitored by thermoouple pled inside the groove of the flnge in lose proximity of the smple. The dp ws obtined by Monte- Crlo simultion tehnique using the ode SRIM 000 [3]. 3

4 X-ry diffrtion: A Philips PW1710 X-ry diffrtometer ws used to reord X-ry intensities sttered from the exmined smples. Copper k α (wvelength λ= Å) rdition (40kV, 40 ma) ws used s n X-ry soure. Smples were snned in step-sn mode (0.0 /step) over the ngulr rnge (θ) of 15 to 70. X-ry diffrtion dt were olleted for.5 se t eh step. Resistivity mesurement: Resistivity t room temperture of the smples were mesured using four probe tehnique with HP 340A nnovoltmeter with resolution of 0.1 nv nd Keithley 4 progrmmble urrent soure. 1 ma urrent ws employed. Method of nlysis: Studies of morphous mterils represent lrge nd importnt emerging re of mterils siene. It is n re whih is not menble to the most of the onventionl theoretil tehniques of solid-stte physis s there is no periodiity to simplify the mthemtis. Due to the lk of periodiity, extrtion of struturl informtion from morphous mterils beomes very diffiult. In this work we hve used XRD tehnique to nlyze the vritions of the struturl prmeters of morphous rbon due to irrdition. XRD is very useful nd simple tehnique to understnd the struturl detils of the solid-stte substnes. Inident X-ry interts with lrge volume of the mteril t time nd n verge property of the mteril n be hrterized rther thn the lol property. This mkes XRD powerful tehnique for studying the disordered mterils whih is inherently heterogeneous nd where the estimtion of verge property hs got prtil signifine. 4

5 Fig. 1 shows typil XRD profile for the unirrdited smple A. The brod peks nd the diffused nture of the XRD profile indite the presene of disorder in the smple [4]. The first pek of the profile orresponds to the (00) pek of the ordered hexgonl grphite struture. While the seond pek orresponds to the (100) nd (101) peks, whih is often lled the (10) bnd. Before rrying out ny nlysis the diffrtion profiles were orreted for polriztion nd bsorption using the tehniques desribed in the literture [4,5]. Fig. shows typil normlized orreted intensity urve [Curve A] for the unirrdited smple A plotted ginst s sinθ s = long with λ the oherent sttering [Curve B], the inoherent Compton sttering [Curve C] nd the totl independent sttering i.e. sum of the urves B nd C [Curve D]. Sine the observed intensity urve in Fig. 1 n be ffeted by mny rndom ftors, suh s smple pking, it n not be used diretly either for quntittive nlysis or for omprison of spetr of the smples irrdited with different doses. To eliminte these problems, the intensity ws onverted to eletroni units by normlizing the profile with suitble ftor so tht t lrge s the normlized urve [Curve A] osilltes bout the Curve D [4,6,7]. The redued intensities [4,6] of the smples: I=i(s)= A C B were then lulted from the normlized orreted intensities. Fig. 3 shows the typil redued intensity plot ginst s for the unirrdited smple A. Further quntittive nlysis is bsed on this redued intensity profile rther thn the observed one. Frtion of morphous rbon: The (00) pek of the smple in the observed diffrtion profile (Fig. 1) is lmost t the sme position s tht observed in rystlline lyered hexgonl grphite struture 5

6 [PDF# 75161]. However, it is diffused nd brodened inditing tht the smple exists in form whih is intermedite between the morphous nd the rystlline sttes [4,8]. These types of strutures re built up from the individul grphite lyers rrnged prllel to one nother slightly greter the norml grphite sping (rystlline) but rndom in trnsltion prllel to the lyer nd rottion bout the norml (morphous) [8] nd known s rndom lyer lttie struture. Hene, the diffrtion pttern of suh mteril onsists of two types of refletions rystlline type refletions nd diffuse two dimensionl lttie refletions (morphous ontribution). Therefore the redued intensity ( I ) n be expressed s the sum of two seprte ontributions from the rystlline rbon ( I Cr ) nd the morphous rbon ( I m ), I = I Cr + I m. (1) The frtion of morphous rbon does not ontribute to the pek intensity nd is only refleted in the bkground of the intensity pttern. Aording to Frnklin [5] the intensity ontributed by the morphous rbon is onstnt over the whole sttering rnge nd equl to the frtion of the morphous rbon (x A ). Thus, the redued intensity n be expressed s I = I Cr + x A. () For the first pek of the diffrtion pttern i.e. for (00) refletion, the bove intensity eqution n be written s I = I 00 + x A (3) Wrren theoretilly lulted the intensity equtions for rndom lyer ltties in terms of the lyer dimension nd the position of the relted rystlline refletion [8]. Applying 6

7 Wrren results in se of rbon Frnklin [5] found out the expression for the redued intensity of the (00) refletion s I = s n p n sin ( πnd ( nsin ( πd n s) s)) n (4) Where d n is the inter-lyer sping on the groups of N prllel lyers, nd p n is the frtion of the totl rbon ontined in suh groups. It is obvious from the intensity eqution tht the frtion of the rbon, whih does not tke prt in the lyer struture, does not ontribute to the (00) bnd. Aording to our ssumption the frtion of rystlline rbon (lyered struture) present in the smple is ( 1 x A ). Thus the tul redued intensity due to (00) refletion redues to I 00 = ( sin ( πndns) 1 x A) pn s n ( n sin ( πdns)) (5) Using this in Eq. (3) we rrive t I 1 x x A A s = n p n sin ( πnd ns) ( nsin ( πd s)) n (6) The right-hnd side of the bove eqution is periodi polynomil expression with the mximum ourring t d s i i n mx = i (ny integer). Its first mximum ours t d nsmx = 1. This pek orresponds to the (00) bnd in the redued intensity urve. Sine eh item in this polynomil expression, onsequently the summtion is symmetril round the mximum s i mx, the left hnd side of the eqution should hve the sme symmetril profile. This ft hs been exploited to determine the frtion of morphous rbon ( x A ) in the smples [5]. The expression in the left-hnd side of the Eq. (6), ( I x )/( 1 x ) ( s / ) A A, is very sensitive to x A. 7

8 To determine the frtion of morphous rbon in the smples the expression ( I x )/( 1 x ) ( s / ) is lulted from the redued intensity (I) nd plotted s A A funtion of s. x A is vried to obtin the best symmetril plot of ( I x )/( 1 x ) ( s / ) vs. s by fitting Loretzin urve. Fig. 4 shows typil A A most symmetri plot of ( I x )/( 1 x ) ( s / ) vs. s for the unirrdited smple A A A for x A =0.76. This vlue of x A orresponds to the frtion of morphous rbon in the smple [5]. The s vlue orresponding to the mximum of the plot ( s i mx ) is obtined from the fit. Assuming tht the inter-lyer sping is the sme for ll size groups nd equl to the men inter-lyer sping of the rystlline struture ( d 00 ) we get the lttie i sping d 00 from the reltion d 00 smx = 1. Averge stking height nd rystlline dimeter: XRD is the most ommon nlytil tehnique used for determining the struture of ordered nd disordered rbons [5,9-1]. Ordered grphite hs the hexgonl struture (spe group P6 3 /mm) with rbon lyers hving the ABAB-stking long the -xis, lthough rhombohedrl 3R grphite with ABCABC-stking is lso possible. Disorder n our due to vriety of resons, inluding the presene of lol 3R stking, rndom shifts between djent lyers, unorgnized rbons whih re not prt of lyer struture, nd strin in the lyers. These disorders ffet the ordered grin size L nd L long - xis nd -xis respetively. L nd L n be pproximtely lulted from the (00) nd (10) bnd respetively using n empiril expression first derived by Sherrer [13,14], whih is 8

9 Kλ L = (7) B osθ Where B nd θ orresponds to the full width t hlf mximum (FWHM) nd the position of the pek respetively. K is onstnt depending on the refletion plne nd equls to 0.89 nd 1.84 for (00) bnd (10) bnd [15-18] respetively. Results nd Disussions Mny studies hve been mde on the effet of hevy ion irrdition in rystlline mterils. On the ontrry very few litertures n be found on the irrdition effet in morphous mterils. In this work we hve extensively studied the irrdition effet used by swift hevy ion on two sets of morphous rbon smples. The rdition dmge in the smples is ssyed by the dmge energy deposition using displements of toms. The d 00, L nd L vlues obtined for the unirrdited nd the irrdited smples re listed in Tble 1. The estimted size of ordered grins in both the smples is found to derese long -xis, but remins lmost unffeted long the -xis s funtion of dose. The d 00 vlues lso did not hnge muh due to irrdition. The onstny of d 00 vlues nd the derese of L with the dose of irrdition suggest tht the sping of the lmellr plnes of hexgonl struture of grphite did not hnge due to irrdition but their orienttions with respet to eh other got rndomized. L nd L mesure the long rnge order of these lmellr strutures long nd xis respetively. The onstny of L nd the redution of L with the irrdition n be ttributed to the ft tht the presene of the strong ovlent (σ nd π) bonding long the -xis nd the wek vn der Wls bonding long the -xis. The hnge in the frtion of morphous rbon in the smples due to inresing dose of irrdition is shown in Fig. 5. It is seen 9

10 tht the frtion of morphous rbon in smple A grdully inresed due to irrdition. In se of smple B, the frtion of morphous rbon hs inresed substntilly t initil doses but there is some inrese of ordering t the highest dose of irrdition. Fig. 6 nd 6b shows the vrition of L nd L with the frtion of morphous rbon for the smples A nd B respetively. It is seen tht for both the smples L nd L vry linerly with the frtion of morphous rbon. The frtion of morphous phse present in the smples is mesure of the degree of disorder in it. The liner dependene of L nd L lerly demonstrtes tht L nd L n lso be mesure of the disorder. The rnge of 145 MeV Ne 6+ ion in the smples is 143 µm. The kineti energy of the inident projetile (Ne 6+ ) is primrily deposited on the trget by ioniztion nd nuler energy loss. The mesured eletril resistivities of the smples were of the order of 10-4 Ωm. This is quite ppreible to quenh the ioniztion used by irrdition lmost instntneously. Hene, it my be rgued tht the observed inrese of disorder in the smple due to irrdition did not use due to ioniztion but due to nuler energy loss. Neon being hevy ion, trnsfers suffiient kineti energy to the primry knok on toms whih in turn produe displement sdes. As the primry knok on proeeds through the smple, loosing energy in suessive ollisions, the displement rosssetion inreses [19]. This displement of toms inresed the disorder in the smples. For the highest dose ( Ne 6+ /m ) of irrdition the dmge is found to be dp, s lulted from SRIM 000 [3]. The smple B is more rystlline in the unirrdited stte. During irrdition, suffiient mount of energy is trnsferred in the system for eletroni exittion nd formtion of defets. During deexittion of 10

11 eletrons, enormous mount of energy dissiption (roughly times higher thn the stored energy) leds to disordering upto ertin dose. But, t the highest dose, the export of entropy is so high tht it my exeed the internl entropy prodution nd leds to redution of the totl entropy of the system [0]. This n result in ordering in the sense of sttistil thermodynmis nd the frtion of morphousity omes down. This ordering effet under irrdition t high doses is explined s self-orgnized phenomenon in the literture [1, ]. Moreover, it is seen tht the behvior of the rboneous smples under irrdition is dependent on the nture of the preursor used for prepring these smple. The proess nd preursor dopted for mking smple A, with high frtion of morphous rbon, is more suitble for the use s modertor in therml nuler retors s it is seen tht the frtion of morphous rbon hs inresed with irrdition reduing the possibility of Wigner energy storge. Conlusions Two sets of novel morphous rbon mterils re irrdited with high-energy Ne 6+ ions nd the struturl prmeters of the unirrdited nd irrdited smples re estimted by XRD profile nlysis. The frtion of morphous rbon is generlly found to inrese with the irrdition dose for both the smples. The estimted vlues of the d 00 nd L did not hnge muh due to irrdition. The estimted vlues of L orroborte with the inrese of disorder in both the smples with the inresing dose of irrdition. 11

12 Referenes 1. R.E. Nightingle: Nuler Grphite, Ademi Press, New York, Grphite Modertor Lifeyle Behvior, IAEA- Tedo- 1996, vol. 901, pp J.P. Biersk, L.G. Hggmrk: Nul. Instrum. Meth., 1980 vol. 174, pp. 57, The stopping nd rnge of Ions in Mtter (SRIM 000) softwre developed by J. Ziegler nd J.P. Biersk is vilble t the website 4. H.P. Klug, L.E. Alexnder : X-ry diffrtion proedures for polyrystlline morphous mterils, nd ed. John Wiley, New York, 1974, pp R. E. Frnklin: At Cryst., 1950, vol. 3, pp B.E. Wrren: X-ry diffrtion, Addision-Wesley, Reding(MA), N. S. Gingrih: Rev. of Mod. Phys, 1943, vol. 15, pp B.E. Wrren: Phys. Rev., 1941, vol. 59, pp S. Ergun: Chemistry nd Physis of Crbon, Mrel Dekker, New York, 1968, vol. 3, pp S. Ergun: Crbon, 1976, vol. 14, pp M.S. Dresselhus, G. Dresselhus: Adv. Phys., 1968, vol. 30, pp W. Rulnd: Chemistry nd Physis of Crbon, Mrel Dekker, New York, 1968, vol. 4, pp B.D. Cullity: Elements of X-ry diffrtion, Addision-Wesley, 1978, pp P. Sherrer: Nhr. Ges. Wiss. Gottingen, 1918, vol., pp J. Bisoe, B.E. Wrren: J. Appl. Phys., 194, vol.13, pp T.F. Yen, J.G. Erdmn, S.S. Pollk: Anl. Chem. 1961, vol. 33, pp

13 17. Y. Kshiwy, K. Ishii: ISIJ Int., 1991, vol. 31, pp J.V. Dubrwski, W.W. Gill: Ironmking Steelmking, 1984, vol. 11, pp R.W. Weeks, R. O. Sttergood, S. R. Pti: J. Nul. Mter., 1970, vol. 36, pp F. Bnhrt: Rep. Prog. Phys., 1999, vol. 6, pp A. Seeger: Rd. Eff. Deffts Solids, 1989, vol. 111/11, pp A. Seeger, W. Frnk: Solid Stte Phenomen, 1988, vol.3/4, pp

14 Tble 1. Vrition of d 00, L nd L with the irrdition dose. Dose Smple A Smple B (Ne 6+ /m ) d 00 (Å) L (Å) L (Å) d 00 (Å) L (Å) L (Å) Unirrdited (4) 7.7(4) (3) 8.(3) () 7.3() () 7.8(4) () 7.5(3) (3) 7.5(3) (3) 7.0(3) () 7.7(4) 14

15 Figure Cptions: Fig. 1. XRD profile of the unirrdited smple A. Fig.. Normlized orreted intensity urve [Curve A] for the unirrdited smple A long with the vrition of the oherent sttering [Curve B], the Compton sttering [Curve C] nd the totl independent sttering [Curve D] ginst s. Fig. 3. Redued intensity urve for the unirrdited smple A Fig. 4. Determintion of frtion of morphous rbon ( x A ) in the unirrdited Smple A. Fig. 5 Vrition of frtion of morphous rbon with the irrdition dose. Fig. 6 Vrition of L nd L with the frtion of morphous rbon. 15

16 3000 Intensity in Arbitrry Units θ in Degree Fig. 1. XRD profile of the unirrdited smple A. 16

17 60 Normlized Intensity in E.U B D A 10 C s Fig.. Normlized orreted intensity urve [Curve A] for the unirrdited smple A long with the vrition of the oherent sttering [Curve B], the Compton sttering [Curve C] nd the totl independent sttering [Curve D] ginst s. 17

18 3.5 Redued Intensity sinθ/λ Fig. 3. Redued intensity urve for the unirrdited smple A 18

19 (I-x A )*s /(0.0606*(1-x A )) (00) profile lulted from mesured Redued intensity Lorentzin fitting s=sinθ/λ Fig. 4. Determintion of frtion of morphous rbon ( x A ) in the unirrdited Smple A. 19

20 Frtion of Amorphous rbon (%) Smple A Smple B x x x10 14 Dose (Ne 6+ /m ) Fig. 5 Vrition of frtion of morphous rbon with the irrdition dose. 0

21 1 () L L 10 L, L (Angstrom) (b) L L Frtion of morphous rbon (%) Fig. 6 Vrition of L nd L with the frtion of morphous rbon. 1

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