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Defects and Short-Range Order in Nepheline Group Minerals: a Silicon-29 Nuclear Magnetic Resonance Study

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Defects and Short-Range Order in Nepheline Group Minerals: a Silicon-29 Nuclear Magnetic Resonance Study Phys Chem Minerals (1986) 13: 371-381 PHYSIC8 CHEMIS]RY I MINERA © Springer-Verlag 1986 Defects and Short-range Order in Nepheline Group Minerals: a Silicon-29 Nuclear Magnetic Resonance Study J.F. Stebbins 1, J.B. Murdoch 2, I.S.E. Carmichael a, and A. Pines 4 1 Department of Geology, Stanford University, Stanford CA 94305, USA 2 Technicare Corporation, P.O. Box 5130, Cleveland, OH 44101, USA 3 Department of Geology, University of California, Berkeley, CA 94720; and Earth Sciences Division, Lawrence Berkeley Laboratory, Berkeley, CA 94720, USA 4 Department of Chemistry, University of California, Berkeley, CA 94720; and Materials and Molecular Research Division, Lawrence Berkeley Laboratory, Berkeley, CA 94720, USA Abstract. 29Si magic-angle spinning nuclear magnetic reso- fore often difficult to interpret and apply thermochemical nance (NMR) spectra are presented for seven crystalline data for these materials, or to understand precisely the rela- phases of the nepheline group: natural nephelines from a tionships between observed structure and thermal history plutonic environment (Bancroft, Ontario) and a volcanic in both nature and the laboratory. In one example of con- deposit (Mt. Somma, Italy), kalsilite, synthetic pure Na cern to the present authors, Stebbins et al. (1984) presented nepheline, carnegieite, and two samples of orthorhombic systematic relationships between the entropies of fusion of KA1SiO4. In all phases, nearly all of the Si sites have four minerals and the field strengths of the non-framework cat- A1 neighbors, indicating nearly complete A1-Si ordering. ions. One potentially interesting comparison is between Excess Si over the 1:1 stoichiometric Si/Al ratio appears nepheline and anorthite, both tectosilicates with the same to substitute randomly for A1 on an ordered lattice, adding Al/Si ratio but different charge balancing cations. The com- Si sites with 3 and 0 A1 neighbors in a 3:1 ratio. Various parison was uncertain because of the unknown structural types of structural disorder, including A1-Si disorder, that state of the latter: either the two entropies were approxi- are reported from some x-ray diffraction studies are prob- mately equal (if nepheline is disordered at melting), con- ably long range in nature and are due to the presence of trary to the pattern seen in many other minerals, or the ordered domains. entropy of fusion for anorthite was significantly larger, as In naturally occurring nepheline, the relative abundance expected with its more highly charged cation. of T sites with three-fold local symmetry is maintained at Nuclear magnetic resonance (NMR) spectroscopy has the ideal stoichiometric value of 1/4, even when the K/(K+ recently been used to help understand tectosilicate mineral Na) ratio is substantially lower. This is in agreement with structures, especially of zeolites and feldspars (e.g. Putnis conclusions reached about the average structure from x-ray and Angel (1985); Kirkpatrick et al. 1985; Fyfe et al. 1983; data. The distinction between the two sites, at least in terms Vega 1983; Lippmaa et al. 1980 and 1981). The technique of the local structure that is reflected in 29Si NMR chemical is a good complement to x-ray diffraction, as it is sensitive shifts, is lost in a pure Na nepheline sample. primarily to local electronic environments instead of long- range geometry. Direct structural information can therefore be obtained independently of the averaging effects of dis- order and pseudosymmetry. Separate NMR spectra can also be measured for isotopes of many of the major constit- Introduction uents of silicates, such as 2aNa, 27A1, 170, and 29Si. Minerals close in composition to the NaA1SiO4-KA1SiO4 It is not yet possible, however, to rigorously calculate binary (the nepheline group) are common in silica-under- the NMR spectra of solids of known structure and composi- saturated igneous rocks such as syenites and phonolites and tion. This results from the complex shielding effect of chem- their metamorphic equivalents. Their synthetic analogs ical bonding and electronic configurations on the local mag- have also long been of interest to ceramists and materials netic fields experienced by nuclear spins. Progress in the scientists. The phases are all tectosilicates, and are made theoretical prediction of NMR chemical shifts is being up of open, three dimensional frameworks of SiO4 and made (Tossell 1984; Tossell and Lazzareti 1985; Engle- A10~ tetrahedra, with Na, K, and Ca as interstitial charge- hardt and Radeglia 1984), but interpretation of spectra balancing cations. As for pure crystalline SiO2, the minor is still largely limited to (sometimes precise) empirical corre- energy differences between structures with slightly different lations and (generally qualitative) simple, general informa- Si-O-(A1,Si) bond angles (Gibbs et al. 1981) and the tion about the influences of structure. great topological variety of networks of corner-shared tetra- In spite of this problem, 295i NMR has been of great hedra lead to an intriguing number of polymorphs related value in mineralogy. In particular, the technique of magic by either reconstructive or displacive phase transitions. Be- angle spinning (MAS) NMR has been used to obtained cause of the complexity of these transitions, and the diffi- high-resolution spectra of solids: the broadening effect of culty of characterizing aluminum-silicon ordering by x-ray the anisotropic part of the chemical shielding tensor is re- techniques on often finegrained, highly twinned materials, moved by rapid rotation at the "magic" angle (54.7 °) with the detailed crystal structures of some of the low-tempera- respect to the magnetic field (Andrew 1981). Because the ture, low-symmetry forms are not known exactly. It is there- spin-l/2 29Si nucleus is spherical, there are no complications 372 caused by nuclear quadrupole coupling to electronic field high pressure phases can be quenched. Higher order transi- gradients. The resulting spectra are relatively straightfor- tions, which involve only bond bending and minor displa- ward to interpret from empirical relationships. The isotro- cive shifts that lead to symmetry changes, are rapid, and pic 298i chemical shift fi (the relative shift in resonant fre- high temperature phases are generally unquenchable. Many quency from that of a reference compound, typically tetra- nepheline group minerals also undergo displacive transi- methylsilane) is very sensitive to the local chemical environ- tions that during cooling produce low temperature struc- ment of the Si atom. The value of fi has been shown to tures with relatively low symmetry and complications such depend on several interrelated structural variables, which as multiple twinning. Unfortunately, the fine grain size of include the average Si-O-(A1,Si) bond angle around an some of these materials makes single-crystal x-ray studies Si, the mean bond strength around the cation, the average impossible. In these cases, heat capacity and phase transi- distance to neighboring tetrahedral cations, the number of tion data such as those reported by Lange et al. (1986) surrounding oxygens bound to other tetrahedral units (i.e. on the samples studied here can be a very important part the extent of polymerization of the anionic structure), and of sample characterization. the number of those tetrahedral neighbors that are A104 Various types of disorder occur in nepheline group min- instead of SiO 4 groups (Smith and Blackwell 1983; Ram- erals. In both kalsilite and nepheline, the oxygen atoms das and Klinowski 1984; Mfigi et al. 1984; Smith et al. whose mean positions are on the trigonal axis (O1) appear 1983; Grimmer and Radeglia 1984; Lippmaa 1980). The to actually be distributed among three sites slightly dis- latter relationship has played a major role in the determina- placed from the axis (e.g. Hahn and Buerger 1955; Perotta tion of the Si-A1 ordering and site distribution in complex and Smith 1965). The positions of at least some of the zeolite structures (e.g. Fyfe et al. 1982, 1983), information other atoms in the structure are probably coupled to that that could probably be obtained in no other way. of O1 as well, as the tetrahedra rotate more-or-less as units It must be emphasized that A1-Si distributions deter- away from ideal symmetry (Simmons and Peacor •972). mined by 29Si NMR are related to the local structure that Relatively large uncertainties in all atomic positions are affects individual Si sites. This may be quite different from therefore common in x-ray structure refinements. Occupan- the long range, average structure observed by x-ray diffrac- cies of the three O1 positions, and presumably the three tion. In particular, it is possible (and perhaps even common) sets of tetrahedral orientations, are randomly mixed on a for a crystal structure to be made up of small domains, small but unknown scale, even in untwinned single crystals. each of which has a high degree of short-range order. If McConnell (1962) and other workers have suggested the ordering sequence of these domains varies through a that nepheline and related minerals are made up of domains crystal, however, the material may exhibit little or no long- with ordered O1 atoms. A number of different types of range order. Short range order can have major effects on boundaries between such domains are possible. If they are thermodynamic properties: McConnell (1985) has pointed abundant enough, some of these should be directly detect- out that the entropy changes of many order-disorder phase
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