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Orientation of Exsolved Pentlandite in Natural and Synthetic Nickeliferous

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Orientation of Exsolved Pentlandite in Natural and Synthetic Nickeliferous AmericanMineralogist, Volume61, pages913-920, 1976 Orientationof exsolvedpentlandite in naturaland synthetic nickeliferous pyrrhotite Cenr A. FRANCISI,MtcHesl E. FLestz, KuL,q MlsnA.8,AND JenrEs R. Cnntcl rDepartment of Geological Sciences, Virginia Polytechnic Institute and State Uniuersity, Blacksburg, Virginia 24061 2Department of Geology, The Uniuersity of Western Ontario, London, Ontario N6A3K7 sDepartment of Geological Sciences, The Uniuersity of Tennessee,Knoxuille, Tennessee37916 Abstract Pentlandite(pn), (Fe, Ni)rSB,exsolves from nickeliferouspyrrhotite (po), (Fe, Ni)r-,S, in the form of flamesexhibiting weak reflectionanisotropism and preferredorientation. X-ray precessionstudies on both natural and syntheticcrystals have establishedthe orientation relation:(111)pnll (00.1)po; (0Tl )pn ll (l 1.0)po;(TT2)pn ll (10.0)po.In synthesisexperiments, rapidlyquenched samples of (Fe,Ni)r-,Ssolid solutions contain randomly oriented blebs of pentlandite,whereas slowly cooled charges contain coherent lamellae of pentlanditeparallel to (00.1)of pyrrhotite. Introduction typical Sudbury-typeFe-Ni sulfideassemblages lie within the monosulfidesolid-solution field at higher Threetextural varieties of pentlandite,(Fe,Ni)156, temperatures(Naldrett and Kullerud, 1967;Craig are common in the pyrrhotite-bearing(Sudbury- and Kullerud, 1969) further supportsthis inter- type) naturalnickel sulfide assemblages: (l) massive pretation.Thus the subsolidusexsolution origin of (blocky) pentlandite,often containingislands of pentlanditein nickel-sulfideassemblages is well es- pyrrhotite;(2) partialto completerims of pentlandite tablished. aroundpyrrhotite grains; and (3) stringersand blebs The presentcontribution is thecombined report of of pentlanditein pyrrhotiteoften showingpreferred two independentinvestigations, one on a natural orientation."Flame" or "brush" texture,consisting sampleby MEF andKCM andthe other on synthetic of fine subparallelplates or needleswith sharp to materialby CAF andJRC. The crystallographic rela- raggedborders, is characteristicof the latter variety tionshipbetween host pyrrhotiteand exsolvedpent- of pentlandite(Fig. l), but it alsooccurs at the mar- landite is established,correcting previous reports, ginsof rim-typeand (morerarely) blocky pentland- and structuralcontrols on the exsolutionprocess are ite, projectinginto the adjacentpyrrhotite. All these discussed. textural varietiesare often found within the limits of Orientedintergrowths of severalore-mineral pairs a singlepolished section; however, detailed electron- wereexamined by Gruner (1929),who recognizeda microprobeanalyses have failed to establishany sys- commonstructural feature in them.The arrangement tematiccompositional differences among them. of atomsin one or more atomiclayers of the first is Crystallizationof pentlanditeduring cooling nearlyidentical with that in oneor morelayers of the of synthetichigh-temperature (Fe,Ni)r-,S (mon- second.Further, a singleelement, usually oxygen or osulfide)solid solutions(Newhouse, 1927; Hewitt, sulfur, populatesthose layers. For example,there is a 1938;Hawley and Haw, 1957;Kullerud, 1956,1962), closedimensional fit betweenthe oxygenpositions in often with texturestypical of naturalpyrrhotite-pent- the close-packed(lll) layersof magnetiteand those landite assemblages,strongly suggests that the pent- in the close-packed(00.1) layers of ilmenite.Such an landitein naturalassemblages has exsolved from a arrangement,like that of coherenttwin boundaries, high-temperaturenickeliferous pyrrhotite. The with- tendsto minimizeinterfacial energy because the first drawalof themonosulfide solid-solution (mss) solvus coordinationspheres of the atomson the common in the Fe-Ni-S systemto progressivelymore S-rich planeare satisfied by both structures(Buerger, 1943; compositionsat decreasingtemperature (Naldrett, e/ 194s). al.,1967;Shewman and Clark, 1970; Misra and Fleet, Gruner (1929)concluded on the basisof crystal- 1973a),and the fact that the bulk compositionsof the structuralarguments that true "orientedintergrowths 913 914 FRANCIS.FLEET, MISRA AND CRAIG pyrrhotite exsolvedfrom pentlandite.In the former example,"cut parallelto the base"[presumably the (00.1)of pyrrhotitel,pentlandite occurs in threedis- tinct orientationsresembling a snowflake.In thelater example,apparently hexagonal-shaped pyrrhotite crystalslie in the (l I l) planeof pentlandite.Ehren- bergalso described the only knownexample of pent- landiteepitaxially overgrown on pyrrhotite(Fig. 2). Pentlanditeoccurs as tri-radiateovergrowths in two orientationson the (00.1)face of pyrrhotitewith the rays extendingperpendicular to the {10.0}form of pyrrhotite.These "stars" are composed of smallcrys- tals that havefaces normal to the ray directionsand henceparallel to i10.0)of the pyrrhotitesubstrate. Assumingthat the three-foldsymmetry of the stars was not merelyinherited from the substratebut ac- tually representsthat of [1I l] of pentlandite,Ehren- bergassigned the smallvertical faces to the dodecahe- dron,{l l0}.He thusdeduced that the (ll l) and(l l0) planesof pentlanditeparallel the (00.1)and (10.0) planes of pyrrhotite respectivelyli.e. ( 1I 1) pn ll(00.1)poand (110)pn ll (10.0po1. Orientedintergrowths of pentlanditeand pyrrho- FIG I Photomicrographs illustrating some typical pentlandite (pn)-pyrrhotite (po) textural relationships. The bar in each photo- micrograph represents0.04 mm. Oil immersion, reflected light. (a) Stringer of flame-textured pentlandite (light gray) in pyrrhotite (darker gray). Note the preferred orientation of the flames parallel to the pyrrhotite cleavage.Specimen 52, Falconbridge mine, Sudbury, Ontario, Canada. (b) Oriented blebs of flame pentlandite (light gray) in pyrrhotite (darker gray). Specimen9868, Creighton mine, Sudbury, On- tario, Canada. of pentlandite and pyrrhotite . are improbable if not impossible," despiteprevious reports of such in- tergrowths by Newhouse (1927) and others. Sub- sequently Lindqvist et al. (1936) showed that the pentlandite structure determined by Als6n (1925), which formed the basis of Gruner's argument, was incorrect;that structureassumes a unit-cetlcomposi- tion of 8(FeNirSn)and has the S and metal positions reversed relative to the acceptedstructure. Responding to Gruner's paper, Ehrenberg (1932) pentlandite documentedoriented intergrowths of and Frc. 2. Pentlandite epitaxially overgrown on pyrrhotite (vertical pyrrhotite. His polishedsections from Sudbury show dimension2.5 mm) from Miggiadone bei Pallanza,Piemont, Italy both pentlandite exsolved from pyrrhotite and (from Ehrenberg, 1932, with permission). ORIENTATION OF EXSOLVED PENTLAN DITE 915 off-setvery slightlyfrom the crossedposition. A reex- aminationof otherpolished sections from the earlier studiesconfirms that weak anisotropismis a charac- teristic feature of the flame pentlandite,and to a lesserextent, of the smallergrains of rim-typepent- landitein theseassemblages. When muchof the en- closingpyrrhotite is removed,the anisotropismis markedly reduced,suggesting that it results from elasticstrain. Such pentlandite is likely to havepre- servedits originalorientation relationship with the host pyrrhotiteand wastherefore considered ideal for the presentstudy. A small fragment(about 0.01 mm in longestdi- Frc. 3. Photomicrographof flame-texturedpentlandite (light mension)of an intergrowthof pyrrhotiteand flame grey) in pyrrhotiteshowing distinct anisotropism. Analyzer 2o off pentlanditewas removed from a polishedsection of crossedposition, oil immersion,reflected light. Bar is 0.04 mm. specimen9868 and examinedby the precession Specimen9868, Creighton mine, Sudbury, Ontario, Canada. method.A representativeX-ray diffractionpattern is shownwith an interpretationof the cerltralarea of tite arecommonly encountered in experimentalprod- this photographin Figure 4. The verticalreciprocal ucts as well as in natural samples.They werefirst latticerow in Figure4a includesboth pyrrhotite(po) producedexperimentally by Hawleyand Haw (1957) 00./ and pentlandite(pn) hhh diffractions,thus con- andhave subsequently been reproduced by a number of workers(e.9. Naldrett et al. 1967;Misra, 1972: Craig,1973). The crystal structuresof both pentlanditeand high-temperaturepyrrhotite are now well-known. High-temperaturepyrrhotite, which is the iron end- memberof the mss,has the NiAs structure(Harald- sen,1941). Lundqvist (1947) confirmed that the mss alsohas the NiAs structure.Pentlandite was shown to be isostructuralwith CoeSe,by Lindqvistet al. (1936)on the basisof powdermethods. The structure was confirmedby Pearsonand Buerger(1956) and Knop and lbrahim(1961), and has since been refined by Rajamaniand Prewitt(1973). Experimentalmethods and results Natural samples The specimensused in this portion of the in- vestigationwere polishedsections from earlier elec- tron-microprobestudies of naturaf pentlanditeas- semblages(Misra and Fleet, 1973a,1974). More detailed examination of the assemblagefrom the Creightonmine, Sudbury(Specimen 9868) reveals that the flame pentlanditehas a weak but distinct reflectionanisotropism (Fig. 3) with parallel ex- tinction. As far as we are aware, anisotropic pentlanditehas not beenreported in the literature. precessionphotograph This anisotropismis often maskedby the Ftc. 4n. Zero level showingthe crystal- much lographicorientation of pyrrhotite and exsolvedpentlandite in strongeranisotropism ofthe enclosingpyrrhotite, but specimen9868. [01.0]po, [10]pn precessionaxis; p = 20o:Zr- is readilyrecognized when the microscope analyzer is filteredMoKa
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