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High-Pressure Crystal Chemistry of Cubanite, Cufers

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High-Pressure Crystal Chemistry of Cubanite, Cufers American Mineralogist, Volume 77, pages 937-944, 1992 High-pressure crystal chemistry of cubanite,CuFerS, CarnnnrNr McClvrmoNr* JrNvrrN ZruNG, RonBnr M. HlznNo Llnnv W. FrNcBn GeophysicalLaboratory and Centerfor High-PressureResearch, Carnegie Institution of Washington, 5251Broad Branch Road NW, Washington,DC 20015-1305,U.S.A. ABSTRACT We have studied cubanite, CuFerS, (orthorhombic, space gtoup Pcmn, a: 6.46, b : 11.10, c : 6.22 A), using single-crystalX-ray diffraction in a diamond-anvil cell at room temperature from 0 to 3.68 GPa. Refinementswere performed aI 0, 1.76, and 3.59 GPa, and cell parameterswere measuredat 20 pressuresup to 3.68 GPa. The linear compress- ibilities of the a, b, and c crystalaxes are 0.00513(5),0.00479(5),and 0.00575(4)GPa ', respectively.Compressibility data were fitted to a Birch-Murnaghan equation of statewith parametersKo : 55.3 + 1.7 GPa with Ko' constrained to be 4. High-pressurerefinement data indicate that the principal responseof the crystal structure to compression is a re- duction in Cu-S bond lengths, whereasFe-S bond lengths remain essentiallyunchanged. Results are compared to bulk moduli and polyhedral bulk moduli of other sulfides. INrnonucrroN lography provides an excellent means for examining the effect of pressure on individual atomic configurations. The crystal structure of cubanite, CuFerSr, is ortho- Cubanite is a worthy candidate becauseof the interest in rhombic with ordered tetrahedral cation sites and S at- the effect ofpressure on intervalence transitions (see,for oms in approximately hexagonal closest packing. The example,Burns, I 98 l) and becausevery few sulfideshave structure was first determined by Buerger (1945, 1947) beenexamined with this technique.We undertook a crys- and described as slices of wurtzite structure parallel to tallographic study of cubanite at high pressurewith the (010) with widthb/2,joined such that every other slab is following goals: (l) to determine the relative axial com- inverted, resulting in edge-sharedpairs oftetrahedra. The pressibilities and bulk modulus of cubanite, (2) to ob- valenceof Cu has been establishedas * I on the basis of serve changesin cation-anion configurations with pres- neutron diffraction data (Wintenberger et al., 1974), sure through variations in bond lengths,bond angles,and whereasFe atoms appearto occupy adjacent edge-shared tetrahedral geometries,and (3) to examine the effect of tetrahedra as Fe2*and Fe3*,with rapid electron exchange pressrueon the electron structure of Fe, basedon changes betweenthem. Crystal structure refinementsindicate cen- in the atomic arrangements. trosymmetric spacegroup Pcmn, which implies that the two Fe atoms are in identical oxidation statesacross the ExprnrlrnNTAr, METHoDS centerof symmetry on a time-averagedbasis (Fleet, I 970; Roorn conditions experiment Szymanski, 1974). Mtissbauerspectra show only one site for Fe from 4.2Klo room temperature(Imbert and Win- A single crystal of cubanite was selectedfrom sample tenberger,1967; Greenwood and Whitfield, 1968),which R17907 (Morro Velho, Nova Lima, Brazil) provided by is consistent with Fe atoms in the same valence state on the National Museum of Natural History, Smithsonian the time scaleof the Mdssbauereffect (1.5 x l0-' s). Institution, Washington, DC. A rectangular prismatic From neutron diffraction data, Wintenbergeret al. (1974) cleavagefragment, approximately 30 x 60 x 100 pm, found a singleFe moment of 3.2 p,",consistent with rapid was used for the X-ray diffraction experiments. Data on electron exchange.Electrical resistivity data of Sleight and a crystal mounted in air were obtained with a Rigaku Gillson (1973) have shown that cubanite is a semicon- AFC-5 goniometer with a rotating anode generator pro- ductor, implying that rapid electron exchangeis confined viding MoKa radiation with a graphite monochromator, -9 -15 to pairs of edge-sharedtetrahedra. ourro (sin0)/)\: 0.1/A,with < h < 9, = k < < Goodenough (1980) has shown that the edge-shared 15, and 0 < / 8. The 212,212, and 060 reflections configuration of Fe tetrahedra should stabilize the Fe2*- were monitored as intensity and orientation standards Fe3*configuration. An interesting problem, therefore, is every 150 reflections; their intensities varied by up to the efect ofpressure on electrontransfer, sincethe crystal l.5olofrom the mean. A total of 2138 symmetry-allowed structure will inevitably change. High-pressure crystal- reflections were measured,of which 1504 were observed at I > 2or. Unit-cell parameters were determined from the positions of24 centeredreflections in the range 3l < * Presentaddress: Bayerisches Geoinstitut, Postfach l0 12 5 I, 20 < 39. Absorption correctionswere made with the Ag- W-8580 Bayreuth, Germany. nost program supplied as part ofthe diffractometer con- 0003404x/ 92109l 04937$02.00 937 938 MCCAMMON ET AL.: CUBANITE CRYSTAL CHEMISTRY TABLE1. Refinementconditions and refined parameters of cubanite at several pressures 0 GPa in air 0 GPa in cell 1.7GPa 3.6 GPa Number of observations(, > 2o) 479 180 166 IAR R(%l 22 c.u 4.6 4.6 Weighted R (%) 29 ao 8.3 7.6 Extinction,r- (x 105) 4.0(21 5.4(5) 5.2(s) 0.6(1) Atom Parameter Cu x 0.5836(1) 0.5827(12) 0.5834(13) 0.5831(1 2) v V4 th V4 t/4 z 0.1227(11 0.1209(7) 0.11 68(7) 0.11 14(7) B 1.49(1) 1 90(10) 2.06(e) 1.67(9) Fe x 0.41479(8) 0.4124(9) 0.4118(9) 0.4066(9) v 0.41293(4) 0 4124(3) o.4127(2\ 0.4132(2) z 0.63664(7) 0.6377(s) 0.633s(4) 0.629e(5) B 0.92(1) 1.26(8) 1.50(7) 1.32(7) S1 x 0.58s7(4) 0 5e6(6) 0.5e6(6) 0.611(5) v Y4 V4 V4 z 0 7577(2) 0.7595(12) 0.7556(10) 0.7s03(11 ) B 0.96(3) 1.55(28) 1.43(26) 1.67(34) S2 x 0.4116(2) 0.4080(30) 0.4124(34) 0.4245(29) v 0.41545(8) 0.4158(8) 0.4151(7) 0.4146(8) z 0.26703(11) 0.2657(7) 0.2621(7) 0.2564(7) B 0.se(2) 1.42(15) 1.66(1 s) 1.19(1 6) trol software. Equivalent reflections were averagedin point refinements, furthermore, relied on reflections within a glovp mmm to give 681 unique reflections,of which 479 relatively narow 20 runge, from l8 to 33o, in order to with 1 > 2or were used for structure solution and refine- reduce systematic errors associatedwith measuring lat- ment. tice parameters at different 20 ranges (Swanson et al., l 985). High-pressure experiments In an effort to improve pressurecalibration, the pres- The single crystal (30 x 60 x 100)rrm studied at room sure cell was opened, and the cubanite crystal was re- pressurewas mounted in a diamond-anvil cell designed mounted with a cleavagofragment of calcium fluoride for single-crystal X-ray diffraction studies (Hazen and 100 x 100 x l0 prmthick as an additional pressurestan- Finger, 1982).An Inconel 750X gasketwith a hole 0.35 dard, along with ruby chips. The 2d values of fluorite 220, mm in diameter was centeredover one 1.0-mm diamond 202, and022 reflectionsprovide a sensitiveinternal pres- anvil, and the crystal was centered on the face with a sure standard(Hazen and Finger, l98l). Unit-cell param- small dot of the alcohol-insoluble fraction of Vaseline eterswere measuredat an additional l2 pressuresto 3.68 petroleum jelly. We used a mixture of 4:l methanol to GPa, and pressureswere measuredby both ruby and cal- ethanol as the hydrostatic pressuremedium, and several cium fluoride methods. At severalpressures only calcium l0 pm fragmentsof ruby were sprinkled near the crystals fluoride pressureswere obtained, owing to the failure of for internal pressurecalibration. Special care was taken the laser in the ruby calibration system. to ensure that a clearance of 0.1 mm was maintained When comparing unit-cell parametersat several pres- betweenthe crystalsand gasketwall. This precaution pre- sures,it is important to employ the sameset of reflections vents significant X-ray shadowing of the crystal by the for each measurement.Cell refinements at all presswes gasketwall. were determined with the same set of eight reflections: All high-pressureX-ray data were obtained on a Huber 440, 042, 033, 403, 442,442,460, and 270 (the eight automated four-circle difractometer with graphite Friedel pairs are also included by the eight-reflectioncen- monochromatized MoKa radiation. Unit-cell parameters tering routine). for the crystal were measuredat six pressuresto 3.6 GPa Intensity data were obtained for the cubanite at 0.0, with the procedure of King and Finger (1979), whereby 1.76, and 3.59 GPa, prior to the inclusion of the calcium several reflections are measured in eight equivalent ori- fluoride internal pressure standard. The rectangular entations. This procedure minimizes errors associated cleavagefragment of cubanite was mounted with the c with crystal centering and diffractometer alignment. All axis approximately perpendicularto the flat diamond fac- TABLE2. Anisotropicthermal parameters ( x 103) for cubaniteat room conditions R A P22 v23 UU e-51(15) 3.2s(5) 8.2s(14) 0 0 0 Fe s.53(11) 1.74(3) 6.27(10) -0.06(6) 0.37(10) 0.10(5) al 5.86(44) 1.79(9) 6.63(26) 0 0 0 S2 6.17(25) 1.s8(6) 6.18(15) -0.06(19) -0.43(17) -0.51(8) McCAMMON ET AL.: CUBANITE CRYSTAL CHEMISTRY 939 Tnele 3, Cubaniteanisotropic thermal ellipsoids at room con- TeeLe5. Selectedinteratomic distances and anglesfor cubanite ditions at severalpressures Rms 0 GPa 0 GPa Angle with respect to '1.7 amplitude Parameter in air in cell GPa 3.6 GPa Axis (A) Cu tetrahedron 1 0.127(1) 90 90 0 Cu-Sl 2.271(1) 2.250(1) 2.22s(9) 2.209(10) 0.142(1) 0 90 90 Cu-S1 2.295(3) 2.249(35) 2.23(4) 2.12(3) 3 0 142(1) 90 0 90 Cu-S2 [2] 2.327(1) 2.338(13) 2.306{13) 2.242(12) I 0.103(1) 65(10) 34(11) 11 1(6) Mean Cu-S 2.305(1) 2.294(1) 2.268(5) 2.203(51 2 0.107(1 )
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