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1.
New equilibrium experiments have been performed in the 20–27 kbar range to determine the upper thermal stability limit of endmember deerite, Fe 12 2+ Fe 6 3+ [Si12O40](OH)10. In this pressure range, the maximum thermal stability limit is represented by the oxygen-conserving reaction: deerite(De)=9 ferrosilite(Fs)+3 magnetite(Mag)+3 quartz(Qtz)+5 H2O(W) (1). Under the oxygen fugacities of the Ni-NiO buffer the breakdown-reduction reaction: De=12 Fs+2 Mag+5 W+1/2 O2 (10) takes place at lower temperatures (e.g. T=63° at 27 kbar). The experimental brackets can be fitted using thermodynamic data for ferrosilite, magnetite and quartz from Berman (1988) and the following 1 bar, 298 K data for deerite (per gfw): Vo=55.74 J.bar-1, So=1670 J.K-1, H f o =-18334 kJ, =2.5x10-5K-1, =-0.18x10-5 bar-1. Using these data in conjunction with literature data on coesite, grunerite, minnesotaite, and greenalite, the P-T stability field of endmember deerite has been calculated for P s=P H 2O. This field is limited by 6 univariant oxygenconserving dehydration curves, from which three have positive dP/dT slopes, the other three negative slopes. The lower pressure end of the stability field of endmember deerite is thus located at an invariant point at 250±70°C and 10+-1.5 kbar. Deerite rich in the endmember can thus appear only in environments with geothermal gradients lower than 10°C/km and at pressures higher than about 10 kbar, which is in agreement with 4 out of 5 independent P-T estimates for known occurrences. The presence of such deerite places good constraints on minimum pressure and maximum temperature conditions. From log f O 2-T diagrams constructed with the same data base at different pressures, it appears that endmember deerite is, at temperatures near those of its upper stability limit, stable only over a narrow range of oxygen fugacities within the magnetite field. With decreasing temperatures, deerite becomes stable towards slightly higher oxygen fugacities but reaches the hematite field only at temperatures more than 200°C lower than the upper stability limit. This practically precludes the coexistence deerite-hematite with near-endmember deerite in natural environments.  相似文献   

2.
Fe57 Mössbauer spectra were measured on compositions of the series Fe1?x/3Ta1+x/3O4, 0≤x≤1. The spectra are characterized by mixed valencies of Fe2+ and Fe3+ ions for 0<x<1. Starting from x=0 with rutile structure, a trirutile structure forms towards x=1. Quadrupole splitting QS of Fe3+ is QS(Fe3+)≈0.55 mm/s and isomer shift IS is IS(Fe3+)≈0.40 mm/s (referred to Fe); both quantities exhibit minor variations along the series. The Fe2+ subspectra for x>0.5 were fitted using one symmetrical doublet; however, for x<0.5 two symmetrical doublets were necessary to describe these patterns. QS(Fe2+)=2.0–3.2 mm/s and IS(Fe2+)=0.90–1.15 mm/s for all compositions. In the case x<0.5, marked temperature dependent QS values appear to exist. This feature may be related to short range order effects and possibly also in part to intervalence electron transfer betwee Fe2+ and Fe3+ ions.  相似文献   

3.
The color and spectroscopic properties of ironbearing tourmalines (elbaite, dravite, uvite, schorl) do not vary smoothly with iron concentration. Such behavior has often been ascribed to intervalence charge transfer between Fe2+ and Fe3+ which produces a new, intense absorption band in the visible portion of the spectrum. In the case of tourmaline, an entirely different manifestation of the interaction between Fe2+ and Fe3+ occurs in which the Fe2+ bands are intensified without an intense, new absorption band. At low iron concentrations, the intensity of light absorption from Fe2+ is about the same for E∥c and E⊥c polarizations, but at high iron concentrations, the intensity of the E⊥c polarization increases more than ten times as much as E∥c. This difference is related to intensification of Fe2+ absorption by adjacent Fe3+. Extrapolations indicate that pairs of Fe2+-Fe3+ have Fe2+ absorption intensity ～200 times as great as isolated Fe2+. Enhanced Fe2+ absorption bands are recognized in tourmaline by their intensity increase at 78 K of up to 50%. Enhancement of Fe2+ absorption intensity provides a severe limitration on the accuracy of determinations of Fe2+ concentration and site occupancy by optical spectroscopic methods. Details of the assignment of tourmaline spectra in the optical region are reconsidered.  相似文献   

4.
Deerite, Fe 12 2+ Fe 6 3+ [Si12O40](OH)10, thus far known from ten localities in glaucophane schist terranes, was synthesized at water pressures of 20–25 kb and temperatures of 550–600 °C under the of the Ni/NiO buffer. The X-ray powder diagram, lattice constants and infrared spectrum of the synthetic phase are closely similar to those of the natural mineral. A solid solution series extends from this ferri-deerite end member to some 20 mole % of a hypothetical alumino-deerite, Fe 12 2+ Al 6 3+ [Si12O40](OH)10. The upper temperature breakdown of ferri-deerite to the assemblage ferrosilite +magnetite+quartz+water occurs at about 490 °C at 15 kb, and 610 °C at 25 kb fluid pressure for the of the Ni/NiO buffer. Extrapolation of these data to lower water pressures indicates that deerite can be a stable mineral only in very low-temperature, high-pressure environments.  相似文献   

5.
The heat capacity of synthetic ferrosilite, Fe2Si2O6, was measured between 2 and 820 K. The physical properties measurement system (PPMS, Quantum Design®) was used in the low-temperature region between 2 and 303 K. In the temperature region between 340 and 820 K measurements were performed using differential scanning calorimetry (DSC). The C p data show two transitions, a sharp λ-type at 38.7 K and a small shoulder near 9 K. The λ-type transition can be related to collinear antiferromagnetic ordering of the Fe2+ spin moments and the shoulder at 10 K to a change from a collinear to a canted-spin structure or to a Schottky anomaly related to an electronic transition. The C p data in the temperature region between 145 and 830 K are described by the polynomial $C_{p} {\left[ {\hbox{J\,mol}^{{ - 1}}\,{\hbox{K}}^{{ - 1}} } \right]} = 371.75 - 3219.2T^{{ - 1/2}} - 15.199 \times 10^{5} T^{{ - 2}} + 2.070 \times 10^{7} T^{{ - 3}} $ The heat content [H 298 – H 0] and the standard molar entropy [S 298 – S 0] are 28.6 ± 0.1 kJ mol?1 and 186.5 ± 0.5 J mol?1 K?1, respectively. The vibrational part of the heat capacitiy was calculated using an elastic Debye temperature of 541 K. The results of the calculations are in good agreement with the maximum theoretical magnetic entropy of 26.8 J mol?1 K?1 as calculated from the relationship 2*Rln5.  相似文献   

6.
Zusammenfassung Die Kristallstruktur von künstlichem Voltait, K2Fe5 2+Fe3 3+Al[SO4]12· ·18 H2O, kubisch hexakisoktaedrisch,Fd3c–O h 8,a 0=27,254 ,Z-16, wurde mittels photographischer Röntgendaten bestimmt. Die Aufklärung der Struktur erfolgte mit Patterson- und Fouriermethoden unter Zuhilfenahme des multiplen isomorphen Ersatzes. Die Verfeinerung nach der Methode der kleinsten Quadrate ergab mit anisotropen Temperaturfaktoren für 726 beobachteteF hkl R=0,033. Das Hauptmerkmal der Struktur ist ein 3dimensionales Gerüst aus [Fe3+O6]-Oktaedern, [Fe 5 6/2+ Fe 1 6/3+ O4(H2O)2]-Oktaedern und [K+O12]-Polyedern, die durch SO4-Tetraeder verknüpft werden. Hohlräume dieses Gerüstes werden von ungeordnet orientierten [Al(H2O)6]-Oktaedern eingenommen. Es wird gezeigt, daß Al als wesentlicher Bestandteil dieses Voltaits angesehen werden muß.
The crystal structure of voltaite, K2Fe5 2+Fe3 3+Al[SO4]12·18H2O
Summary The crystal structure of synthetic voltaite, K2Fe5 2+Fe3 3+Al[SO4]12· · 18 H2O, cubic hexakis-octahedral, space groupFd3c–O h 8,a 0=27.254 ,Z=16, was determined from photographic X-ray data. The structure was solved by Patterson and Fourier-methods with the aid of multiple isomorphic substitution. Least squares refinement with anisotropic temperature factors resulted inR=0.033 for 726 observedF hkl . The dominant structural feature is a continous framework composed of [Fe3+O6]-octahedra, [Fe 5 6/2+ Fe 1 6/3+ O4(H2O)2]-octahedra and [K+O12]-polyhedra linked by SO4-tetrahedra. The arrangement gives rise to cages occupied by disordered [Al(H2O)6]-octahedra. It is shown that Al must be considered to be a essential constituent of such voltaites.

Mit 2 Abbildungen  相似文献   

7.
An in situ high pressure X-ray diffraction study on synthetic pure ilvaite powder has been performed using a diamond anvil cell. A phase transition from monoclinic to orthorhombic (Pbnm) has been observed at 2.25 Gpa, which can be described as a λ-transition.  相似文献   

8.
The formation of the solid solution series MgCO3-FeCO3 in the system Mg2+-Fe2+-CO 3 2? -Cl 2 2? -H2O has been investigstad between 200° C and 500° C. The experimental results show that the composition of any of these carbonates strongly depends on the temperature: At high temperatures mixed crystals rich in MgCO3 are formed and low temperatures lead to the formation of FeCO3-rich carbonates. Thus, at 200° C a Fe-poor (Mg-rich) solution is in equilibrium with a Fe-rich carbonate. At temperatures higher than 350° C a Fe-rich (Mg-poor) solution coexists with a Fe-poor (Mg-rich) solid phase; see Fig. 1. At 350° C a solution with a mole fractionmFe2+/(mFe2++mMg2+) of 0.20 leads to the formation of magnesite very poor in Fe, whereas at 250° C the same solution is in equilibrium with sideroplesit, containing 80 Mol-% FeCO3, see Figs. 2 and 3. The importance of the experimental results for the formation of deposits of magnesite and siderite is discussed.  相似文献   

9.
 Magnetic measurement of Fe3− x Si x O4 spinel solid solutions indicates that their Curie temperatures decrease gradually, but not linearly, from 851 to 12 K with increasing content of nonmagnetic ions Si4+. Magnetic hysteresis becomes more noticeable in solid solutions having a larger content of Fe2SiO4. Saturation magnetizations of Fe3− x Si x O4 samples increase up to x=0.357 and they are easily saturated in the field of H=0.1 T. However, magnetization of the sample of x=0.794 does not approach saturation even at high field of H=7.0 T and has a large coercive force. The Si4+ disordered distribution is confirmed to be tetr[Fe3+ 1− x + x t Si4+ x (1− t )] octa[Fe2+ 1+ x Fe3+ 1− x − x t Si4+ x t ] O4 by the spin moment, which is consistent with site occupancy obtained from X-ray crystal structure refinement. Their molecular magnetizations would be expressed as M B={4(1+x)+10xt}μB as functions of composition parameter x and Si4+ ordering parameter t of the solid solution. The sample of x=0.794 is antiferromagnetic below the Néel temperature, mainly due to the octahedral cation interaction M O–M O, while both M T–M O and M O–M O interactions induce a ferrimagnetic property. Concerning magnetic spin configuration, in the case of x>0.42, the lowest dɛ level becomes a singlet, resulting in no orbital angular momentum. Received: 20 April 2000 / Accepted: 11 September 2000  相似文献   

10.
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11.
The distribution of Fe3+ and Ga3+ between the two tetrahedral sites in three synthetic melilites has been studied by using 57Fe Mössbauer spectroscopy. In the melilite, (Ca2Ga2SiO7)50 (Ca2Fe3+GaSiO7)50 (mol %), the distribution of Fe3+ and Ga3+ in T1 and T2 sites is apparently random, which can be explained in terms of the electrostatic valence rule. However in the melilites, (Ca2MgSi2O7)52 (Ca2Fe3+GaSiO7)42 (Ca2Ga2SiO7)6 and (Ca2MgSi2O7)62 (Ca2Fe3+GaSiO7)36 (Ca2Ga2SiO7)2 (mol %), Fe3+ shows preference for the more ionic T1 site and Ga3+ for the more covalent T2 site. If the electronegativity of Ga3+ is assumed to be larger than that of Fe3+, the mode of distribution of Fe3+ and Ga3+ can be explained in terms of our previous hypothesis that a large electronegativity induces a stronger preference for the more covalent T2 site.  相似文献   

12.
 The adiabatic elastic moduli of polycrystalline En50Py50 and En80Py20 majorite-garnet solid solutions (where En=4MgSiO3, Py=Mg3Al2Si3O12) and the end-member En100 tetragonal majorite were determined at ambient conditions using Brillouin spectroscopy. The adiabatic bulk modulus, K, and shear modulus, μ, of En50Py50 were found to be K=173.1 (20) and μ=92.3 (10) GPa, and are indistinguishable from those of the end-member pyrope, Py100. The moduli of the more majorite-rich samples are significantly lower and are virtually identical to each other (K=162.6(11) and μ=85.7(7) for En80Py20; K=166(5) and μ=88(2) for En100). In combination with previously reported moduli for this system, we conclude that both K and μ are constant over the compositional range from Py100 to a majorite content of about 70–80%, whereupon the moduli decrease substantially. For compositions ranging from En80Py20 to the end-member majorite, the moduli are also approximately independent of composition, but at a lower value. An alternative model with a continuous decrease in moduli with increasing majorite content cannot be excluded, within the uncertainties of existing measurements. The contrast in moduli between aluminous pyrope garnet and Al-free majorite are small compared with the modulus changes accompanying the pyroxene – majorite phase transformation. Received August 16, 1995 /Revised, accepted January 12, 1996  相似文献   

13.
Reduction of Fe3+ to Fe2+ by heating in hydrogen reduces the absorbance of the bands at 9,000 and 13,800 cm?1 in the E ⊥ c spectrum of tourmaline, and the 9,000 and 11,000 cm?1 bands in the E ∥ (001) spectrum of biotite. This behaviour is consistent with the presumed d-d origin of these bands (which seems well established) only if they gain much of their intensity from exchange-coupling with neighbouring Fe3+ ions. Intensification of spin-forbidden bands in sapphire by Fe3+-Fe3+ exchange-coupling was recognized by Ferguson and Fielding (1971, 1972), but exchange-coupling has not previously been thought to intensify spin-allowed d-d bands. Spin-allowed exchange-coupled bands resulting from Fe2+-Fe3+ pairs have features in common with both normal single ion d-d bands, which they resemble in energy, width and pressure dependence, and Fe2++Fe3+→Fe3++Fe2+ charge transfer bands, which they resemble in temperature-, heat treatment-, composition-, and polarization-dependence. Distinction between normal d-d, charge transfer, and pair d-d absorptions is thus complicated, and criteria for assigning these bands are discussed. Spin-allowed exchange-coupled pair bands should be sought in the spectra of transition metal clusters (trimers and polymers as well as pairs may be involved) whenever geometry favours their origin. It is possible that the bands near 10,000 and 11,500 cm?1 in blue sapphire, and at about 5,000 cm?1 in titanian garnets are of this type, but many other examples are likely to occur. Exchange-coupling may involve ions other than Fe3+ (e.g., Mn2+, also d 5), although Fe2+-Fe2+ coupling is unlikely to be important at laboratory temperatures.  相似文献   

14.
Single crystals of Li-aegirine LiFe3+Si2O6 were synthesized at 1573?K and 3?GPa, and a polycrystalline sample suitable for neutron diffraction was produced by ceramic sintering at 1223?K. LiFe3+Si2O6 is monoclinic, space group C2/c, a=9.6641(2)?Å, b= 8.6612(3)?Å, c=5.2924(2)?Å, β=110.12(1)° at 300?K as refined from powder neutron data. At 229?K Li-aegirine undergoes a phase transition from C2/c to P21 /c. This is indicated by strong discontinuities in the temperature variation of the lattice parameters, especially for the monoclinic angle β and by the appearance of Bragg reflections (hkl) with h+k≠2n. In the low-temperature form two non-equivalent Si-sites with 〈SiA–O〉=1.622?Å and 〈SiB–O〉=1.624?Å at 100?K are present. The bridging angles of the SiO4 tetrahedra O3–O3–O3 are 192.55(8)° and 160.02(9)° at 100?K in the two independent tetrahedral chains in space group P21 /c, whereas it is 180.83(9)° at 300?K in the high-temperature C2/c phase, i.e. the chains are nearly fully expanded. Upon the phase transition the Li-coordination changes from six to five. At 100?K four Li–O bond lengths lie within 2.072(4)–2.172(3)?Å, the fifth Li–O bond length is 2.356(4)?Å, whereas the Li–O3?A bond lengths amount to 2.796(4)?Å. From 57Fe Mössbauer spectroscopic measurements between 80 and 500?K the structural phase transition is characterized by a small discontinuity of the quadrupole splitting. Temperature-dependent neutron powder diffraction experiments show first occurrence of magnetic reflections at 16.5?K in good agreement with the point of inflection in the temperature-dependent magnetization of LiFe3+Si2O6. Distinct preordering phenomena can be observed up to 35?K. At the magnetic phase transition the unit cell parameters exhibit a pronounced magneto-striction of the lattice. Below T N Li-aegirine shows a collinear antiferromagnetic structure. From our neutron powder diffraction experiments we extract a collinear antiferromagnetic spin arrangement within the a–c plane.  相似文献   

15.
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16.
Synthetic clinopyroxenes of compositions between CaFe3+AlSiO6 and CaFe 0.85 3+ Ti0.15Al1.15Si0.85O6 have been studied by 57Fe Mössbauer spectroscopy. The spectra consist of two doublets assigned to Fe3+ in M1 and T sites. From the area ratios of the doublets the site occupancies of Fe3+ and Al were determined. Si decreases from 1.00 to 0.85 and Al+Fe3+ increases from 1.00 to 1.15 per formula unit with increasing CaTiAl2O6 component of the clinopyroxene. The atomic ratio of Fe3+(T)/Fe3+(total) is 0.11–0.16; 4.5–7.5 percent of the T sites are occupied by Fe3+. Thus the presence of Si-O-Fe3+, Al-O-Fe3+, and Fe3+-O-Fe3+ bonds is expected in addition to Si-O-Si, Si-O-Al and Al-O-Al bonds. However, the possibility of the former bonds being present would be small, because the amount of Fe3+(T) is far less than that of Si and Al. The isomer shift of Fe3+(T) is one of the largest in the values found previously for Fe3+(T) in silicates. It increases with increasing CaTiAl2O6 component and seems to be correlated to the ionic character of the cation — anion bonds calculated from electronegativity. The quadrupole splittings of Fe3+(M1) and Fe3+(T) decrease with the substitution of Fe3+?Ti4+ in the M1 and of Si?Al in the T sites.  相似文献   

17.
Single-crystal Raman spectra of synthetic end-member uvarovite (Ca3Cr2Si3O12) and of a binary solution (59% uvarovite, 41% andradite) have been measured using single crystal techniques. For each of these garnets, 22 and 21 of the 25 Raman modes were located, respectively. The spectra for uvarovite garnets closely resemble those of the other calcic garnets, grossular, and andradite. The modes for uvarovites do not fit into the same trends as established by the other five anhydrous end-member garnets: the high energy “internal” Si–O modes do not depend on lattice constant in uvarovite. They exceed frequencies for both andradite and grossular. This is likely due to the large crystal field stabilization energy of trivalent chromium. The low energy and midrange modes are at similar frequencies to the other calcic garnets.  相似文献   

18.
Summary Sonoraite, FeTeO3(OH)·H2O, is monoclinic,P 21/c, witha=10.984(2),b=10.268(2),c=7.917(2) Å, =108.49(2)°. For 8 formula units per cell the calculated density is 4.179(2) g/cm3; the observed value is 3.95(1) g/cm3. The Supper-Pace automated diffractometer was used to collect 1884 independent reflections which were corrected for absorption. The structure was determined by an automated symbolic addition procedure. It was refined to a residualR of 6.2% using anisotropic temperature factors for the cations and isotropic temperature factors for the oxygen atoms. Chains of octahedra about Fe extend along [101]; edge-sharing pairs of these octahedra are joined by corner sharing. The Fe–Fe distances across the shared edges are 3.05 and 3.20 Å, short enough to suggest magnetic interactions. All but one H2O are involved in the chains. The Te4+ ions have a pseudotetrahedral coordination, with three oxygen ions forming one face of the tetrahedron and the lone electron pair of Te occupying the fourth corner. The O–Te–O average bond angle is 95°. The Fe chains are tied together by Te–O bonds in all three dimensions.
Die Kristallstruktur von Sonorait, Fe3+Te4+O3(OH).H2O
Zusammenfassung Sonorait, FeTeO3(OH)·H2O, ist monoklin, P 21/c, mit den folgenden Zelldimensionen:a=10,984(2),b=10,268(2),c=7,917(2) Å, =108,49(2)°. Mit 8 Formel-Einheiten errechnet man eine Dichte von 4,179(2) g/cm3; die gemessene Dichte beträgt 3,95(1) g/cm3. Das Supper-Pace automatische Diffraktometer wurde zur Sammlung von 1884 unabhängigen Reflexen benutzt, welche für Absorption korrigiert wurden. Die Struktur wurde mit Hilfe eines vollständig automatischen Programms für symbolische Addition bestimmt. Mit anisotropen Temperaturfaktoren für die Kationen und mit isotropen Temperaturfaktoren für die Sauerstoff-Atome wurde ein Residuum von 6,2% erreicht. Ketten von Eisen-Oktaedern erstrecken sich entlang [101]; Oktaeder-Paare mit gemeinsamen Kanten sind über Eckenverknüpfung verbunden. Die Fe–Fe-Abstände über die gemeinsamen Kanten betragen 3,05 und 3,20 Å, kurz genug, um zu magnetischer Wechselwirkung führen zu können. Nur ein H2O-Molekül ist nicht Teil einer Kette. Die Te4+-Ionen befinden sich in pseudotetraedrischer Koordination; drei Sauerstoff-Ionen bilden eine Fläche des Tetraeders, die vierte Ecke wird durch das einsame Elektronenpaar von Te besetzt. Der Mittelwert des O–Te–O-Bindungswinkels beträgt 95° Die Fe-Ketten werden durch Te–O-Bindungen dreidimensional verbunden.

With 3 Figures  相似文献   

19.
The orthopyroxene crystal structure can be viewed as the stacking of alternating tetrahedral and octahedral layers parallel to the (100) plane. Easy glide occurs in the (100) plane at the level of the octahedral layer to prevent breakage of the strong Si-O bonds. Dislocations with c and b Burgers vectors have been activated in (100) by room temperature indentation in an orthoenstatite gem quality single crystal. Investigations in transmission electron microscopy show that the b dislocations (b?9 Å) are not dissociated while the c's (c=5.24 Å) are dissociated into four partials. This result is interpreted by considering the oxygen sublattice as a distorted FCC one. The four c partials are thus Shockley partials bounding three stacking faults. For the two outer ones, synchroshear of the cations is necessary to keep unchanged their sixfold coordination; the oxygen sublattice is locally transformed into a HCP lattice. This accounts for the observed low splitting (?100 Å) of these faults as compared to the median one (?500 Å) which does not affect the oxygen sublattice and does not require cation synchroshear. In a Fe rich orthopyroxene (eulite), semi coherent exsolution lamellae have been studied. Either only c edge dislocations or both b and c edge dislocations occur in the phase boundaries depending upon the thickness of the lamellae. Only the c dislocations are dissociated. From the observed spacing between these mismatch dislocations a crude estimate of the exsolution temperature is proposed T ex ? 700° C.  相似文献   

20.
We have obtained infrared and Raman spectra for garnets synthesized at high (static) pressures and temperatures along the join Mg3Al2Si3O12 (pyrope) — Mg4Si4O12 (magnesium majorite). The vibrational spectra of Mg-majorite show a large number of additional weak peaks compared with the spectra of cubic pyrope garnet, consistent with tetragonal symmetry for the MgSiO3 garnet phase. The Raman bands for this phase show no evidence for line broadening, suggesting that Mg and Si are ordered on octahedral sites in the garnet. The bands for the intermediate garnet compositions are significantly broadened compared with the end-members pyrope and Mg-majorite, indicating cation disorder in the intermediate phases. Solid state 27Al NMR spectroscopy for pyrope and two intermediate compositions show that Al is present only on octahedral sites, so the cation disorder is most likely confined to Mg-Al-Si mixing on the octahedral sites. We have also obtained a Raman spectrum for a natural, shock-produced (Fe,Mg) majorite garnet. The sharp Raman peaks suggest little or no cation disorder in this sample.  相似文献   

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