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Geochemical Journal, Vol.15, Pp. 229 to 243, 1981 229 Geochemical Journal, Vol.15, pp. 229 to 243, 1981 229 A lp h a-re c oil d a m a g e in n a tu r al zir c o n olite a n d p er o v sk ite W . SlNCLAIR and A. E. RlNGWOOD Research SchoolofEarth Sciences,Austraiian National University,Canberra,A.C.T.2600,Australia (R eceived October_13,1980.' Accepted July 20,1981) Zirconolite (CaZrTi207) and perovskite (CaTi03) are key minerals in SY NR OC, a ceramic m aterial developed for the im m obilization of high level nuclear reactor w astes. Wh en these are incorporated in SY NR OC,the long-1ived radioactive actinide elem ents are preferentially partitioned into zirconolite and perovskite which ~re therefore subjected to the effects of alpha-recoil,resulting from the decay ofthese elem ents. These effects have been studied via X-ray and electron diffraction investigations of natural sam ples of zirconolite and perovskite of varying ages and varying uranium and thbrium contents. The sam ples studied have received cum ulative alpha doses ranging from 1.0 X 1018 to I.1 X I020alg. The upper limit corresponds to the alphairradiation which would bereceived by the zirconolite in SY NRO C containing 10 percent ofhigh levelw aste overaperiod of5 X I08years. These studies show that zirconolitesrem ai n crystalline up to and beyond alphadosesof2 X 1019a/g. This dose would have accum ulated in such a SY NROC zirconolite after a million years ofstorage. Elec- tron microscopy revealed th at the grains were com posed of sm all crystalline dom ains w hich possessed the d efect fluorite-type structure. After a dose exceeding that w hich would be received by SY N ROC in 1OO m illion years,zirconolites appeared m etam ict w hen studied by X-ray diffraction. H owever,the elec- tron microgr.aphsand diffraction patternsclearly dem o nstrate that the m ineral continuesto retain alarge degree of short range order and in no way resem bles a glass. The density changes produced in these zir- conolites byirradiation aresm allandrangefrom Oto 3% atsaturation. P erovskite sam ples which have SY NR OC ages up to 20,000 years decrease in density by I.8:!:0.1%. Their X-ray pow der patterns are essentially unaffected. C om parative studies show thatthe perovskitelat- ticeiseven m oreresistanttothe_effectsofalpha-recoilthanthezirconolitelattice. Theresultsdem onstrate that zirconolite and perovskite are extrem ely resistant to the effectsofnuclearradiation and w illprovide stable crystal stru ctures for the containm entoftheradioactivew asteelem ents duringthetim ere quired for the radioactivity to decay tosafelevels(typically 105-106years). INTRODUCTION em itted by these elem ents, notably neptunium , plutonium , am ericium , and curium isotopes, are Zirconolite (CaZrTi20 7) and perovskite associated with a recoil of the nucleus. The (CaTi03) are used in the SY N R O C process for displacem ents due to the recoil m ay cause do n- the im m obilization of elem ents occurring in siderable day rage to the lattice and decrease the high-1evel nuclear w astes (RlNGW OOD et al., sta bility of the synthetic phases. The al pha 1979). The radioactive w astes are incorp orated emitting elem ents are strongl y p artitioned into into the crystal structures by form ing dilute zirconolite and perovskite and these cry s tals will solid solutions with the SY N R O C phases. The therefore be subjected to m ost of the alpha- w aste elem ents are tightly bound within the recoil dam age. cry stal lattices and are extrem ely resistant to W e have assem bled a collection of naturally leaching by hydrotherm alsolutio ns. occurri ng sam ples of zirconolite and perovskite T hese experim ents, ho wever, do not take containing the alpha em itting elem ents, uranium into consideration the im port ant effects of and thorium . The cum ulative radiation doses nuclear radiation arising m ai nly from alpha- received by these m inerals have been calculated decay ofthe actinide elem ents. Alpha particles and cover a considerable range from I.O X I018 230 W.SlNCLAIR and A.E. RlNGWOOD to I.I X 1020 alphas per gram (O VERSBY and Furtherm ore, the authors support ed the con- RlNGWOOD, 1981). In this paper w e describe clusion that the ability for a m a terialto becom e the effects of increasing doses ofalpha radiation m etam ict was strongly dependent on the cry stal o n the crystal stru ctures of these m inerals using structure. The fact that the m ineralthorianite X-ray diffraction and electron m icroscopy Th02 (w hose fluorite-type structure is the techniques. paren t structure of zirconolite) is not found to R EEVE and W OOLFREY (1980) have ap- be m etam ict in the natural state w as said to be proached the sam e problem by irradiating explained by this hypothesis. SY N R O C mineral assem blages wi th fast neu- COMES et al. (1967) have report ed the ef- trons to sim ulate alpha particle and actinide fects of fast neutron irradiation on single cry stal recoil dam age. Their res ults form a com ple- quartz. These authors observ ed a gradual break- m entary study and will be discussed later. dow n of the structure into a heterogeneous M a ny o ther phases have al so been examined m ixt ure ofcrystalline and m etam ict areas. A fter for the effects of radiation dam age. PYATENKO very strong irr adiation (> I020n/cm 2) the cry stal (1970) has suggested that as m ine rals(including becom es entirely m etam ict and exhibits a dif- zirconolite) becom e m etam ict there is a break- fuse diffraction ring on X-ray photographs. dow n of the cry stal structure leading to a T hey concluded that the Si04 tetrahedra r em ain segregation of new phases on a very sm all scale. nearly undam aged during ir adiation. In con- These new phases m ay represent com ponent trast, the ionic crystal LiF rem ains nearly un- oxide s or a m or e com plex configuration ofions. d ist ort ed w hen subjected to radiation dam age. Extensive studies previously carried out on In view ofthe va riety ofconclusions existi ng zircon (ZrSi0 4) have led to several differi ng in the literature, itseem ed possible that an inde- conclusions. H OLLAND and G OTTFRIED (1955) pendent detailed study on new m ineral types and PE LLA S (1965) invoked a m ultistage p rocess such as zirconolite and perovskite m ay provi de occurring with increasing radiation dose. BuR- necessary inform ation to resolve the effects of SILL and M CL AREN (196 6) have support ed this large doses of nuclear radiation. M oreover, m ultistage process and provided evidence from since these m inerals are key com ponents of electron m icroscopy for the existence of sm all SY N R O C, the inform ation so obtained should crystallites of zircon,even in the m etam ict state. have an im port ant bearing on the long-term PELLAS (1965) concluded that zircon ultim ately behaviour of SY N R O C after incorp oration of decom poses to a m ixture of its com ponent high-level nuclear reactor w astes. oxid e s, Si02 + zr02' W ASILEWSKI et al. (1973) Zi rcon olite, CaZrTi207, is closely related to h ave support ed these conclusions from in frared the d efect fluorite-type (CaF2_*) stru cture absorp ti on spectral studies. (PYATENKO and PUDOVKlNA, 1964; R OSSELL, A lternatively, V ANcE and B OLAND (1975) 1980a, b). It can be derived from the sim ple and V ANCE (1975) have suggested a prog ressive lattice by distortion of the parent cubic cell and disordering of the lattice wi th increasing radia- orde ring of the cations. The stru cture so derived tion dose. These authors did not find a second is m ono clinic and has eight tim es the volum e of new phase for zircons as suggested by H OLLAND the originalcube. and G OTTFRIED (1955) nor the breakdow n of Perovskite (CaTi0 3) is orthorhom bic con- the lattice into its com ponent oxides. Th e con- sistin g of a 3-dim ensional fram ew ork of corn er- clusion of progressive lattice disorder w as also joined Ti06 octahedra with Ca atom s occupying m ade by V ANCE and BOLAND (1978) in studies the spaces betw een them . In nature,perovs kite of Zr02- sh ows a con siderable range o f ioni c su bstitu- M ore recently, CARTZ and FOURNELLE tions. The rare earths an d alkalis com m only (1979) did not observ e a breakdow n of ZrSi04 replace calcium w hile sm allsized cationssuch as into its com ponent oxidesin the m etam ict state. niobium and tantalum replace titanium . Alpha-recoildam age 231 T he ability of these m inerals to accom - containing IO% high level w aste w hich w ould m odate a large range of elem entsin their crystal have received a sim ilar radiation dose. stru ctures is of prim ary im po rtance to their inclusion in the SY N R O C process. EXPERIM ENTAL AND RESULTS 1.1 R adiation dose as a function of S YN R O C A suite of natural sam ples was ex am ined age using X-ray diffraction and electron m icroscopy.
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