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1.
Room temperature and low temperature Mössbauer and optical absorption spectroscopic data on six natural chloritoids characterized by means of electron microprobe and X-ray powder diffraction techniques are presented. Two narrow quadrupole doublets with widths of 0.25–0.29 mm/s assigned to Fe2+ in a relatively large octahedral site and Fe3+ in a smaller octahedral site, are observed in the Mössbauer spectra. Polarized optical absorption spectra reveal three main absorption bands. A broad absorption band at 16,300 cm?1, which is strongly polarized in E‖X and E‖Y and shows a linear increase in integral absorption with increasing [Fe2+] [Fe3+] concentration product, is assigned to a Fe2++Fe3+→Fe3++Fe2+ charge transfer transition. This band displays also a temperature dependence different from that of single ion d?d transitions. Two absorption bands at 10,900 cm?1 and 8,000 cm?1 are, on the basis of compositional dependence and energy, assigned to Fe2+ in the large M(1B) octahedra of the brucite-type layer in chloritoid. Combined spectroscopic evidence and structural and chemical considerations support a distribution scheme for ferrous and ferric iron which orders the Fe2+ ions in the M(1B) octahedra and the Fe3+ ions in the small M(1A) octahedral sites. Both types of octahedra are found in the brucite type layer of chloritoid.  相似文献   

2.
The mixed valence iron silicate ilvaite, CaFe 2 2+ Fe3+Si2O8(OH), displays electron delocalization associated with Fe2+→Fe3+ charge transfer as observed by Mössbauer spectroscopy. Previous studies report the observation of an ‘electron hopping phenomenon’ with resolution of discrete valence states below 320 K. Mössbauer spectra of a suite of naturally occurring ilvaites were recorded over a temperature range, 80 K to 575 K. Five quadrupole doublets were resolved by computer fitting and assigned to Fe2+(A), Fe2+(B), Fe3+(A), and Fe2+(A)→Fe3+(A)‖c and ⊥c. Contrary to prior work, doublets associated with electron delocalization are resolved at 80 K and preclude the use of a Verwey-type order-disorder model. We propose a thermal activation model and discuss its criteria from molecular orbital and mineralogical viewpoints.  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.
Two natural clinopyroxene single crystals were investigated, an aegirine-augite (AEG) and a magnesian hedenbergite (HED). Both samples were carefully characterized by electron microprobe, X-ray diffraction, and Mössbauer spectroscopy. Magnetic susceptibility measurements of powdered samples reveal low temperature antiferromagnetic coupling and Curie-Weiss behaviour with T N =7.5(5)?K, Θ P =?19(1)?K for AEG, and T N =31(1)?K, Θ P =+21(1)?K for HED, respectively. Low temperature Mössbauer spectra exhibit relaxation phenomena. Magnetic susceptibility measurements of the single crystals show the direction of the magnetic moments to be lying within the a/c plane for both samples: 50(±2)° from a and 57(±2)° from c in AEG, and 45(±2)° from a and 60(±2)° from c in HED, respectively. The antiferromagnetic interchain interaction competes with the ferromagnetic intrachain interaction in both pyroxenes. In the magnesian hedenbergite a field induced magnetic transition is found. Its dependence on temperature, magnetic field and crystallographic direction is investigated and described.  相似文献   

5.
The transformation of vivianite and the direct synthesis starting from pure chemicals lead to the formation of lipscombite {Fe x 2+ Fe 3?x 3+ [(OH)3?x/(PO4)2]} with varying Fe2+/Fe3+ molar ratios. The influence of this ratio on the Mössbauer spectra, solubility, electrokinetic potential and infrared spectra has been studied. By means of Mössbauer spectroscopy, the distribution of the Fe2+ and Fe3+ ions between the octahedral sites I and II has been investigated. The unit cell dimensions have been determined from Guinier-Hägg X-ray diffraction patterns. The crystal system is tetragonal for synthetic lipscombite with a=5.3020±0.0005 Å and c=12.8800±0.0005 Å. Lipscombite has been found to show a negative and time-dependent zeta-potential which, moreover, is influenced by the pH of the suspension and the Fe2+/Fe3+ molar ratio. An explanation of the time-dependence of the zeta-potential on variations of solubility is proposed. Infrared absorption spectrum only is characterized by two absorption bands: v OH(3,500 cm?1) and v P?O(1,100-960 cm?1). The density at 25° C is determined in toluene as 3.36±0.01 g·cm?3.  相似文献   

6.
Polarized electronic absorption spectra, E∥a(∥X), E∥b(∥Y) and E∥c(∥Z), in the energy range 3000–5000?cm–1 were obtained for the orthorhombic thenardite-type phase Cr2SiO4, unique in its Cr2+-allocation suggesting some metal-metal bonding in Cr2+Cr2+ pairs with Cr-Cr distance 2.75?Å along [001]. The spectra were scanned at 273 and 120?K on single crystal platelets ∥(100), containing optical Y and Z, and ∥(010), containing optical X and Z, with thicknesses 12.3 and 15.6?μm, respectively. Microscope-spectrometric techniques with a spatial resolution of 20?μm and 1?nm spectral resolution were used. The orientations were obtained by means of X-ray precession photographs. The xenomorphic, strongly pleochroic crystal fragments (X deeply greenish-blue, Y faint blue almost colourless, Z deeply purple almost opaque) were extracted from polycrystalline Cr2SiO4, synthesized at 35?kbar, above 1440?°C from high purity Cr2O3, Cr (10% excess) and SiO2 in chromium capsules. The Cr2SiO4-phase was identified by X-ray diffraction (XRD). Four strongly polarized bands, at about 13500 (I), 15700 (II), 18700 (III) and 19700 (IV) cm–1, in the absorption spectra of Cr2SiO4 single crystals show properties (temperature behaviour of linear and integral absorption coefficients, polarization behaviour, molar absorptivities) which are compatible with an assignment to localized spin-allowed transitions of Cr2+ in a distorted square planar coordination of point symmetry C2. The crystal field parameter of Cr2+ is estimated to be 10?Dq?10700?cm–1. A relatively intense, sharp band at 18400?cm–1 and three other minor features can, from their small half widths, be assigned to spin-forbidden dd-transitions of Cr2+. The intensity of such bands strongly decreases on decreasing temperature. The large half widths, near 5000?cm–1 of band III are indicative of some Cr-Cr interactions, i.e. δ-δ* transitions of Cr2 4+, whereas the latter alone would be in conflict with the strong polarization of bands I and II parallel [100]. Therefore, it is concluded that the spectra obtained can best be interpreted assuming both dd-transitions of localized d-electrons at Cr2+ as well as δ-δ* transitions of Cr2 4+ pairs with metal-metal interaction. To explain this, a dynamic exchange process 2 Crloc 2+?Cr2, cpl 4+ is suggested wherein the half life times of the ground states of both exchanging species are significantly longer than those of the respective optically excited states, such that the spectra show both dd- and δ-δ*-transitions.  相似文献   

7.
The electron paramagnetic resonance (EPR) spectra of Fe3+ in a well cristallized kaolinite from Decazeville in France are well resolved. It is shown that in this sample there are mainly two slightly different spectra, well separated at low temperature and characterized at -150° C by the constants B 2 0 = 0.112 cm?1, B 2 2 = 0.0688 cm?1 for one and B 2 0 = 0.116 cm?1, B 2 2 = 0.0766 cm?1 for the second. These two spectra arise from Fe3+ substituted for Al3+ at the two octahedral positions in equal amounts. The temperature dependence of EPR spectra was studied and was explained by a modification of the octahedral sites.  相似文献   

8.
The influence on the spinel structure of Fe3+ → Cr substitution was studied in flux-grown synthetic single crystals of the magnesiochromite–magnesioferrite (MgCr2O4–MgFe2O4) solid solution series. Samples were analysed by single-crystal X-ray diffraction, electron microprobe analyses, optical absorption and Mössbauer spectroscopy. With the exception of iron-poor samples (3–12 mol-% MgFe2O4), optical absorption and Mössbauer spectra show that iron occurs almost exclusively as trivalent Fe in the present samples. A very intense and broad absorption band at ca 7,800 cm?1 dominates the optical absorption spectra of samples with higher Fe-contents. The appearance of this band is related to a distinct structural disorder of Fe3+ and a development of magnetic ordering as demonstrated by Mössbauer spectra. Profound composition-related changes are observed in the Mössbauer spectra, which are magnetically unsplit in the range 2–41 mol-% magnesioferrite, but become magnetically split in the range 59–100 mol-% magnesioferrite. Structural parameters a 0 and M–O increase with magnesioferrite content and inversion degree, while u and T–O decrease. Our study confirms the previously reported (Lavina et al. 2002) influence of Fe3+ at the M site on T–O bond lengths in the spinel structure.  相似文献   

9.
The cation distribution in the synthetic samples of olivine-type structure with composition (Fe x Mn1?x )2SiO4 was determined at room temperature and confirms previous Mössbauer results. At low temperature an antiferromagnetic ordering is observed. The magnetic structures can be described in the crystallographic cell (i.e. k=0). They are interpreted on the basis of the irreducible representations (modes) of the symmetry groups which are compatible with Pnma. The dominant modes observed for all compounds, including Fe2SiO4 and Mn2SiO4, only differ in their direction. The main direction of magnetization is dominated by the Fe2+ single-ion anisotropy. At 4.2K, for x=0.29, it is parallel to the c-axis, whereas for x=0.76 the direction is parallel to the b-axis. The anisotropy of the M1-sites dominates in the first case, whereas M2-anisotropy dominates in the second case. The influence of temperature is demonstrated for x=0.50 where c is the main direction at 4.2K, when it is b at 38K.  相似文献   

10.
The polarized (E‖a′, E‖b and E‖c) electronic absorption spectra of five natural chromium-containing clinopyroxenes with compositions close to chromdiopside, omphacite, ureyite-jadeite (12.8% Cr2O3), jadeite, and spodumene (hiddenite) were studied. The polarization dependence of the intensities of the Cr3+ bands in the clinopyroxene spectra cannot be explained by the selection rules for the point groups C 2 or C 2v but can be accounted for satisfactorily with the help of the higher order pseudosymmetry model, i.e. with selection rules for the point symmetry group C 3v. The trigonal axis of the pseudosymmetry crystal field forms an angle of 20.5° with the crystallographic direction c in the (010) plane. D q increases from diopside (1542 cm?1) through omphacite (1552 cm?1), jadeite (1574 cm?1) to spodumene (1592 cm?1). The parameter B which is a measure of covalency for Cr3+-O bonds at M1 sites in clinopyroxene depends on the Cr3+ concentration and the cations at M2 sites.  相似文献   

11.
The mixed valence iron silicate deerite, Fe 6 2+ Fe 3 3+ O3[Si6O17](OH)5 whose crystal structure has only recently been fully determined, had been previously examined by both susceptibility measurements and Mössbauer spectroscopy. We reinterpret the Mössbauer measurements from Frank and Bunbury and show that all contradictions between the phenomena, observed in their experiments, and the mineralogical structure disappear when one accepts a thermally activated electron delocalisation associated with Fe2+ ? Fe3+ charge transfer.  相似文献   

12.
Mössbauer spectra were recorded at multiple temperatures between 80 and 293 K to study the nature of Fe3+ in Fe0.05Mg0.95SiO3 perovskite that had been synthesised in a multianvil press at 1650 °C and 25 GPa at its mimimum stability limit. The Mössbauer data were fitted to a model with quadrupole splitting distributions (Fe2+) and Lorentzian lineshapes (Fe3+ and Fen+). The centre shift data were fitted to a Debye model with the following results: ΘM (Fe2+)=365±52 K and ΘM (Fe3+)=476±96 K. Hyperfine parameter data for Fe3+ suggest occupation of the octahedral site only. The average valence seen by the Mössbauer effect in rapid electron exchange that occurs between Fe2+ and Fe3+ is calculated from the hyperfine parameters to be 2.50±0.07. Correction of area fractions for site-dependent recoil-free fractions gives a value for Fe3+/∑Fe of 9.4±1.4%, which is independent of temperature. A perovskite phase of similar composition synthesised in the multianvil press at higher oxygen fugacity gives a value for Fe3+/∑Fe of 16±3%, where Fe3+ appears to occupy both sites in the perovskite structure.  相似文献   

13.
Optical spectroscopy indicated that the partial oxidation of Fe2+ to Fe3+ on heating natural cordierites above ～500° C was not sensitive to oxygen partial pressure. This result suggested that the partial oxidation takes place by loss of mobile charge compensators such as protons. Ionizing radiation also produced partial oxidation of the minor-site Fe2+ to Fe3+, but this effect could be reversed by annealing at ～300° C and so was due only to an electronic redistribution. Mössbauer spectroscopy confirmed these results, although there were complications due to apparent thermal decomposition in localized regions of the cordierites on heating in air. Ionizing radiation also produced strong absorption in the near-ultraviolet and blue regions of the optical spectrum. This absorption, which was strongest in the α polarization, had different annealing characteristics to those of the crystal-field absorption bands near 10,000 cm?1. Dehydration by heating above ～900° C severely reduced the subsequent effect of ionizing radiation on the optical spectra. On heating over a temperature range spanning the dehydration temperature, the lack of any changes in the absorption energies of the β- and γ-polarized crystal field bands near 10,000 cm?1, of any changes in the ratio of the intensities of these β- and γ-polarized crystal field bands, and of any singularity in the intensity variations of the bands with heating temperature, all suggest that these bands originate from substitutional Fe2+ rather than Fe2+ in channel sites. Mössbauer evidence also supports this. The formation of pleochroic haloes in cordierite is discussed briefly. No evidence of CO - 3 centres in the irradiated samples was found.  相似文献   

14.
We investigated a natural Brazilian Fe–Ti-containing andalusite and its thermal behavior by polarized infrared and optical spectroscopy. Polarized infrared spectra of the Brazilian andalusite and their evolution at thermal annealing in air clearly evidence that there are several types of OH-groups in the structure. Optical spectra and their evolution with temperature indicate that the incorporated iron (about 0.43 wt% calculated as FeO) is in the ferrous and ferric state. Incorporation of ferrous iron in the Al-sites of andalusite is discussed as a possible incorporation mechanism for hydrogen. The weakening and disappearance of the Fe2+/Ti4+ IVCT band in the andalusite spectra under annealing in air is caused by oxidization of Fe2+ to Fe3+ in Fe2+/Ti4+ IVCT pairs. The process of oxidation is accompanied by a rearrangement of the hydroxyl groups and dehydration of the sample, especially vivid at the final stage of the thermal annealing at 1,200 °C. During thermal annealing, structural hydroxyls of different types apparently transform into each other: the most distinct are the hydroxyls causing the doublet at 3,516 and 3,527 cm?1 (i.e., H bonded to O1) which seem to transform into the hydroxyls causing the line at 3,461 cm?1 (i.e., H bonded to O2). The infrared spectra scanned across differently colored zones of the crystal clearly show that some amount of hydroxyls is related to Fe2+/Ti4+ IVCT pairs which are the cause of the red-to-black coloration of the sample in E||c-polarized illumination: it is evident that in a part of the hydroxyl groups, OH-vector changes orientation aligning directly along crystallographic a-axis due to some kind of interaction with Fe2+/Ti4+ IVCT pairs.  相似文献   

15.
Laihuite reported in the present paper is a new iron silicate mineral found in China with the following characteristics:
  1. This mineral occurs in a metamorphic iron deposit, associated with fayalite, hypersthene, quartz, magnetitc, etc.
  2. The mineral is opaque, black in colour, thickly tabular in shape with luster metallic to sub-metallic, two perfect cleavages and specific gravity of 3.92.
  3. Its main chemical components are Fe and Si with Fe3+>Fe2+. The analysis gave the formula of Fe Fe 1.00 3+ ·Fe 0.58 2+ ·Mg 0.03 2+ ·Si0.96O4.
  4. Its DTA curve shows an exothermic peak at 713°C.
  5. The mineral has its own infrared spectrum distinctive from that of other minerals.
  6. This mineral is of orthorhombic system; space group:C 2h /5 ?P21/c; unit cell:α=5.813ű0.005,b=4.812ű0.005,c=10.211ű0.005,β=90.87°.
  7. The Mössbauer spectrum of this mineral is given, too.
  相似文献   

16.
Troilite close to FeS, with 0.17 weight percent Cr as main impurity, was obtained from the Agpalilik meteorite. Powder Mössbauer spectroscopy was made in the temperature range 77–645 K. The full Hamiltonian was applied in the fittings. Assuming the asymmetry parameter η to be constant on passing from the high-temperature NiAs-type structure to the medium-temperature MnP-type structure yields a quadrupole splitting (dq=0.5e2 qQ(1+(η2)/3)1/2) value of ?0.25(2) mm/s for these phases. In low-temperature troilite |dq|=0.85 mm/s at room temperature. The combinations of (η, θ, φ) in troilite giving identical spectra range from (0, 49°, -) to (1, 45°, 50°) for negative V zz or from (0.3, 57°, 78°) to (1, 58°, 54°) for positive V zz . Assuming a negative V zz and B‖c gives a θ value in agreement with the shortest Fe-S join being the V zz orientation. The magnetic spin flip of 90° is proposed to occur in the MnP-phase only. The MnP phase-troilite transition occurs at lower temperatures and is more sluggish than in pure FeS.  相似文献   

17.
Manganoan lipscombite (Fe x /2+ , M y /2+ ) Fe 3?(x +y)/3+ [OH)3?(x+y)(PO4)2] was synthesized from pure chemicals. From the study of the Mn2+/Fe2+ atomic ratio by Mössbauer spectra, solubility, and electrokinetic properties, it was found that the crystal structure of lipscombite is not changed substantially by the manganese substitution. The unit cell parameters were determined from Guinier-Hägg X-ray diffraction patterns, which are identical for both synthetic ferrous-ferric and manganoan lipscombite. The two compounds crystallize in the tetragonal system with a=5.3020±0.0005 Å and c=12.8800±0.0005 Å.  相似文献   

18.
Red Fe3+-rich and black Fe3+, Fe2+-rich tourmalines have been studied by optical and Mössbauer spectroscopies to determine the optical characteristics of Fe3+ in tourmaline. Prominent optical absorption features at 485 and 540 nm are assigned to transitions of multiple exchange-coupled Fe3+ pairs in several site combinations. These transitions are more intense than those of isolated Fe3+ and are polarized along the vector between the interacting ions, thus permitting site assignments. The 485 nm band occurs at an unusually low energy for Fe3+ in silicate minerals. Similar behavior has been observed in the spectrum of coalingite, Mg10Fe 2 3+ (OH)24CO3·2H2O, in which Fe3+ occurs in related pairs in edge-shared sheets. These lower energies are proposed to result from magnetic exchange in edge-shared geometries. Antiferromagnetic exchange has been confirmed by a variable temperature magnetic susceptibility study of a Kenyan dravite with 3.36 wt percent Fe. The Mössbauer spectrum of this sample is unusual in that it shows a pronounced decrease in width of component peaks from 298 K to 5 K.  相似文献   

19.
Synthetic ringwoodite γ-(Mg1?x Fe x )2SiO4 of 0.4 ≤ x ≤ 1.0 compositions and variously colored micro-grains of natural ringwoodite in shock metamorphism veins of thin sections of two S6-type chondrites were studied by means of microprobe analysis, TEM and optical absorption spectroscopy. Three synthetic samples were studied in addition with Mössbauer spectroscopy. The Mössbauer spectra consist of two doublets caused by VIFe2+ and VIFe3+, with IS and QS parameters close to those established elsewhere (e.g., O’Neill et al. in Am Mineral 78:456–460, 1993). The Fe3+/Fetotal ratio evaluated by curve resolution of the spectra, ranges from 0.04 to 0.1. Optical absorption spectra of all synthetic samples studied are qualitatively very similar as they are directly related to the iron content. They differ mostly in the intensity of the observed absorption features. The spectra consist of a very strong high-energy absorption edge and a series of absorption bands of different width and intensity. The three strongest and broadest absorptions of them are attributed to splitting of electronic spin-allowed 5 T 2g → 5 E g transitions of VIFe2+ and intervalence charge-transfer (IVCT) transition between ferrous and ferric ions in adjacent octahedral sites of the ringwoodite structure. The spin-allowed bands at ca. 8,000 and 11,500 cm?1 weakly depend on temperature, whilst the Fe2+/Fe3+ IVCT band at ~16,400 cm?1 displays very strong temperature dependence: i.e., with increasing temperature it decreases and practically disappears at about 497 K, a behavior typical for bands of this type. With increasing pressure the absorption edge shifts to lower energies while the spin-allowed bands shift to higher energy and strongly decreases in intensity. The IVCT band also strongly weakens and vanishes at about 9 GPa. We assigned this effect to pressure-induced reduction of Fe3+ in ringwoodite. By analogy with synthetic samples three broad bands in spectra of natural (meteoritic) blue ringwoodite are assigned to electronic spin-allowed transitions of VIFe2+ (the bands at ~8,600 and ~12,700 cm?1) and Fe2+/Fe3+ IVCT transition (~18,100 cm?1), respectively. Spectra of colorless ringwoodite of the same composition consist of a single broad band at ca. 12,000 cm?1. It is assumed that such ringwoodite grains are inverse (Fe, Mg)2SiO4-spinels and that the single band is caused by the split spin-allowed 5 E → 5 T 2 transition of IVFe2+. Ringwoodite of intermediate color variations between dark-blue and colorless are assumed to be partly inversed ringwoodite. No glassy material between the grain boundaries in the natural colored ringwoodite aggregates was found in our samples and disprove the cause of the coloration to be due to light scattering effect (Lingemann and Stöffler in Lunar Planet Sci 29(1308), 1998).  相似文献   

20.
Blanfordite (I), winchite (II), and juddite (III), all showing vivid colors and pleochroism, from highly oxidized parageneses of Indian gondites were studied by microprobe, Mössbauer, and microscope-spectrophotometric techniques and by X-ray structure refinements. The compositions of the Mn-bearing minerals were close to diopsideacmite (I) and magnesio-arfvedsonite to magnesio-riebeckite (II and III). Transition metal ions are located inM(1)-octahedra (I) or predominantlyM(2)-octahedra (II, III). Mössbauer spectra of57Fe(IS, ΔE Q) are typical of octahedral Fe3+ only. Polarized absorption spectra in the UV/VIS/NIR ranges explain color and pleochroism of the minerals. The position of the UV-“edge” is correlated with Fe3+-contents of the minerals, except for judditeE ∥Z, where the edge shows an unusual low energy position. This is most likely due to Mie-scattering of submicroscopic inclusions of braunite with nearly uniform dimensions. In the VIS range, the spectra are dominated by a complex band system between 15,000 and 20,000 cm?1. Energies and ?-values of component bands are compatible with those of Mn3+ d-d transitions in other Mn3+-bearing silicates. The polarization behavior of component bands can best be explained by aC 2(C2″) symmetry of the crystal field. The Jahn-Teller splitting (<9,000 cm?1) of the5 E g ground state of Mn3+ inO h crystal fields is appreciably smaller than in other Mn3+-silicates. Crystal field parameters 10Dq, (I) 13,650, (II) ca. 11,640, and (III) 11,925 cm?1, are near to that in piemontite. The crystal field stabilization energy of Mn3+, (I) 146, (II) ca. 140, (III) 142 \({{{\text{kJ}}} \mathord{\left/ {\vphantom {{{\text{kJ}}} {\text{g}}}} \right. \kern-0em} {\text{g}}}{\text{ - atom}}_{{\text{Mn}}^{{\text{3 + }}} } \) , is appreciably smaller than that found in other Mn3+-silicates (piemontites and manganian andalusites, viridines and kanonaite).  相似文献   

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