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Fullerene and Fullerites. New Modern Materials Yu Fullerene and fullerites. New modern materials Yu. Ossipyan To cite this version: Yu. Ossipyan. Fullerene and fullerites. New modern materials. Journal de Physique IV Proceedings, EDP Sciences, 1994, 04 (C9), pp.C9-51-C9-73. 10.1051/jp4:1994908. jpa-00253468 HAL Id: jpa-00253468 https://hal.archives-ouvertes.fr/jpa-00253468 Submitted on 1 Jan 1994 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. JOURNAL DE PHYSIQUE IV Colloque C9, supplkment au Journal de Physique HI, Volume 4, novembre 1994 Fullerene and fullerites. New modern materials Yu.A. Ossipyan Institute of Solid State Physics, Russian Academy of Sciences, 142432 Chernogolovka, Moscow District, Russia I. Introduction The discovery of a new form of pure carbon - giant molecules called fullerenes and subsequelltly of a new crystalline form of carbon - fullerite crystals - has been a full-scale scientific boom over the past few years. Hundreds of laboratories all over the world are being engaged in synthesizing and studying fullerenes and fullerites and their derivatives, the number of publications amounts to two thousand, and the rate and scope of researches goes 011 growing. This report is not a scientific review and it- is not my aiin to cstablish scientific priorities. This is rather a scientific popular lecture that better fits in with the spirit of this session. In view of this, not to overburden my report, I shall not make individual references in the text and figures since, to be exact and consistent, the number of such references must be very large. At the end of rliy lecture I shall give references to several recent very good reviews devoted to individt~al problenis of fullerene pliysics and chemistry. 'l'he reatlei. will find tile necessary ~xhrenccsto originals in these reviews. 2. History The existence of giant niolecules of carbon, boron or silicon llas loi~gI)eeri hypothized. Individual quantum chemical calculations evidenced for thc possibility of stable AGO, and SO on clusters. 1 know about the results of such calculations made and published ill Moscow back in late 60s early 70s. Possibly, there wcrc Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jp4:1994908 JOURNAL DE PHYSIQUE IV other similar considerations and calculations, however, the ideas and models contained in them were hypothetical and based 011 general though quite sensible, from the stand point of quantum chemistry, assumptions. It was only in 1985 that Richard Smalley's group at Rice University, Texas in collaboration with Harry ICroto at the University of Sussex, England, reported the result of their experimental studies that vapors formed upon laser vaporization of graphite contained considerable amounts of carbon clusters CGO, which was recognized mass-spectrometrically. Concurrently, W.Kratschmer from the Max Planck Institute for Nuclear Physics, Heidelberg, Germany ant1 Donaltl I~luffman, University of Arizona, 'l'ucson and their students 1-.Lamb ancl I<.Fostiropoulos were conccrnctl wifh ~~roducinp, ocarbon smoke, by vaporizing a graphite electrode in an arc discharge in order lo model the carbon state in interstellar dust. Their spectroscopic efforts have shown that <carbon smokes contains CGO clusters which may well contribute to 1K spectrum of interstellar dust. But they asked for more . 1-laving collected the graphite residue resultant from spark erosion at the arc discharge, tliey dissolved it in benzene and, after evaporation of the solution, they got tiny crystals of C60 ant1 C70 mixture, being first man made crystals of citcd works of late has opcnetl avenues for laboratory synthesis of macroscopic amounts of fullercnes crystals, stimulated extensive activity in this field in many laboratories all over the globe. It has opened the new era of various physical and chemical experiments with thcsc novel mk~lcrials. .l'od:~y :I standard technology for synthesizing fullerite crystals involvcs the following stages: graphite vaporization in an inert gas atmosl,licre, one of thc arc tlischargc clcctrotlcs being a graphite rod, collecting tlie vaporization products residue from tlic cha~nbcr walls, dissolving this residue in an organic sol\lent, chromatogral>liic colu1111i separation of solutions of various fractions from each other. Thc solutions are then dried to yield microcrystalline particles (powders) of various CN fractions and, finally, these particles are sublimed to yield CN crystals. It appeared that in the fullerene family CN may be very large -- more than 900, however, most stable and abundant are CGOand C70. The molecular structure of CGOis shown in fig.1. This beautifully symmetric molecule belongs to the icosahedral symmetry and is formed of 12 pentagons and 20 hexagons having the same edge dimensioil close to that of C-C bond in graphite. So, now we know three forms of solid carbon - diamond ifig.2), graphite (fig.3) and fullerite (fig.4). A special interest to studies of physical properties of fullerites was arousctl by pul)licatio~~of the sensational \\rork of the group from AT&T Bell Lab's, who reported an observation of high 'rc (=lot<) superconductivity in fullerite specimens treated in 1)otassiulil vapors. .1. his phenomenon was attributed to the process of potassiunl atoms intcscalatioli inlo lllr crystal lattice interstitial sites of fullcritc, likc it takes place with graphite. I'urtlicl. games with variation of the intercalant's type (of alkali ~netals) resultetl in an increase of .I' up to 301< whic:h, j)rcscntly, is scco~itl only to 'I', values of higll c temperature superco~lductorson the base of copper oxitles. It should be pointed out that the general idea of the niolecular structure of fullerenes, similar to that of aromatic matcrial.~,has suggested that fullcrc,ncs arid fullerites should be inert, chenlically illactive ~natcrials.'l'liis, however, is ~iotlllc case. It has been demonstratccl that f~~llcrcnescan ~)a~.ticil);~tcin ~luliierouscllcrl~ical reactions with the formation of various clicmical deri\!ativcs of fullercnes, 7'his gave birth to a new broad field of organic clicniistrv \\:hic.ll, untloul)tctlly, is ~c~1.y promising. , So, two approaches and, corresponclirlgl,v, t\vo tlit'fcrcnt scientific ficltls call I)(. distinguished in the fullerene a~iclfullerite science: first approacli is to regard fullcritcs 21s stable fornl;~tionsthat Ict atoms of JOURNAL DE PHYSIQUE IV small radius - mainly alkali atoms - intercalate into tlieir interstitial positions. In this case the chemical bonds remain intact in fullerene n~olecules.An investigation of the physical properties of such alkali-doped compounds may be called the fullerene physics of today; second approach concentrates on possible chemical reactions involving break- down of bonds inside the fullerene molecules and formation of derivatives. This province is the fullerene chemistry. Let us discuss these approaches at greater length and consider the principle results obtained. 3. Fullerite physics An important division of this science is structi~ralanalysis of fulleritc crystals. It has necessitated the development of special structural methods related to so-called Rietveld refinement. This method, used in powder diff'ractometry, is basctl on the acception, from rational considerations, of apriori structural motlel ant1 its s~rl)secluc~~~t correction so that tlie positions of all the diffractiorl lines \yere coincident wit11 those derived from model calculations. 'l'o dcfinc reliably structures of various phases of pure and intercalated fullercnes this rncthotl is coml)inecl with a ~nctliodof integral intensity measurements of different X-ray diffraction lines, with Lauc methods to study single crystals, with neutron diffraction and electron diffraction mcthotls. 1) Pure fullerite C60 At room temperature a pure C60 has a crystalline I:CC structure (fig./I), but herewith the niolccules are orientationally disorclcretl tluc 10 tlieir rapitl quasi averaged spinning. In the X-ray time scalc all tlie four molecules of the cubic cell arc structurally equivalent. The lattice parameter a=14,16E compriscs tlie value of the van der Waals molecular diameter I) = 101:. At cooling belo\\! 'I' = 245) - 260 I< the 111 phase transition to a simple cubic lattice (SC) is observed. This transition was documented by different structural methods - powder, on single crystals (X-ray), and, also, neutron and electron diffractions. Differential scanning calorimeter method confirms that the phase transition is a first order. Temperature dependence of C60 molecules spinning characteristics was studied in detail using the NMR on 13c isotope. It was shown that above 140K there was one more phase transitio~l,leading to narrowing of NMR lines (fig.5). Effect of pressure. As the hydrostatic pressure is increased, the self-absorption edge moves to the red spectrum side and the absorption edge shape changes (fig.6). The compressibility modulus of CGO wasdefined from the displacement of the X-ray diffraction lines position under pressure. 2.Intercalated fullerenes As it has been mentioned, an interest to these materials was essentially stimulated by observation of high-T superconductivity in C specimens annealed in C alkali-metal vapors (fig.7). Diffraction and nlorphology studies of C60 speci~ne~~s aged at elevated temperatures in alkali-metal vapors have shown that such treatmerlt gives rise to different phases in thc systenl AxCg. wherc A (Na,l<,Pl),Cs). The following isolated p1lasc.s have been clocnn~eotctl: A2C60 - insulating , A3C60 -- concluctiiig , A4C60 - insulating , A6C60 - insulating , Structural fragments of these phases are shown in fig.8 where large L)alls stand for fullerene CGO molecule and small ones for alkali-metal atoms.
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