X-ray photoelectron studies of titanium in biotite and phlogopite

Evans, Stephen D.; Raftery, E.

doi:10.1180/claymin.1980.015.3.01

Cited by 15 publications

(13 citation statements)

References 20 publications

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“…The technique also requires a reasonably flat exposed crystal surface at least several mm 2 in area. Structural questions concerning isomorphous substitution in micas are thus especially amenable to study in this way (Evans, Adams & Thomas, 1979;Evans, Raftery & Thomas, 1979;Evans & Raftery, 1980a, 1980b, 1982a.…”

Section: Introductionmentioning

confidence: 99%

X-ray photoelectron diffraction studies of lepidolite

Evans

Raftery

1982

Clay miner.

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A B S T R A C T: X-ray photoelectron diffraction data for three cleavage surfaces from a crystal of a Norwegian lepidolite containing 2.3% Rb and 3% Mn are reported and interpreted. Rubidium is shown to occupy anhydrous interlayer sites equivalent to those of potassium, and to be distributed uniformly throughout the crystals. Cleavage occurs in Mn rich regions in which the manganese(II) is located in octahedral sites essentially equivalent to those of lithium. The octahedral A1 sites can readily be distinguished from the Li,Mn sites and it is concluded that AI occupies predominantly M(2), cis sites while Li and Mn(lI) prefer M(1), trans sites. Photoelectron diffraction data also indicate that 40 + 5% of the AI is tetrahedrally coordinated, compared with a figure of ~34% deduced independently from a surface analysis.

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Section: Introductionmentioning

confidence: 99%

X-ray photoelectron diffraction studies of lepidolite

Evans

Raftery

1982

Clay miner.

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“…Analytical data for both micas have been reported previously (Evans & Raftery, 1980a,b, 1982a 10( 0-4 1.6 (lepidolite).…”

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confidence: 59%

“…In the biotite, the major cations do not order but Ti, present at only 1.2~o concentration, preferentially occupies the two cis sites, information which is available uniquely from XPD. Long-range tetrahedral ordering should be detectable by XPD, but was not found in either mica.A few years ago the first detailed X-ray photoelectron diffraction (XPD) studies of mica crystals were reported (Evans et al, 1979;Evans & Raftery, 1980a,b, 1982a; these revealed that XPD could provide information on details of their structure which were difficult or impossible to obtain by established techniques. In particular, information regarding the locations of substitutional ions present at low concentration was accessible (Mn and Rb in lepidolite--Evans & Raftery, 1982a; Ti and Na in biotite--Evans & Raftery, 1980aRaftery, , 1982b, and the direct quantitative determination of the aluminium distribution between tetrahedral and octahedral sites was demonstrated (Evans & Raftery, 1980b).…”

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confidence: 99%

“…In particular, information regarding the locations of substitutional ions present at low concentration was accessible (Mn and Rb in lepidolite--Evans & Raftery, 1982a; Ti and Na in biotite--Evans & Raftery, 1980aRaftery, , 1982b, and the direct quantitative determination of the aluminium distribution between tetrahedral and octahedral sites was demonstrated (Evans & Raftery, 1980b). It was suggested (Evans & Raftery, 1982a) that XPD might also be capable of characterizing cation ordering in micas--some of the data were only readily intelligible on the assumption that cation ordering could produce detectable effects in XPD--but much further work remained to be done.…”

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Cation ordering in lepidolite and biotite studied by X-ray photoelectron diffraction

1987

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A B S T RA C T : Comprehensive X-ray photoelectron diffraction (XPD) studies have revealed octahedral cation ordering in a 1M lepidolite and in a 1M biotite. In the lepidolite (from H~ydaler, Telemark, Norway), all three octahedral sites are differentiated, with Li and Mn concentrated in the trans M(1) site and AI in cis M(3); M(2) contains all three cations. In the biotite, the major cations do not order but Ti, present at only 1.2~o concentration, preferentially occupies the two cis sites, information which is available uniquely from XPD. Long-range tetrahedral ordering should be detectable by XPD, but was not found in either mica.A few years ago the first detailed X-ray photoelectron diffraction (XPD) studies of mica crystals were reported (Evans et al., 1979;Evans & Raftery, 1980a,b, 1982a; these revealed that XPD could provide information on details of their structure which were difficult or impossible to obtain by established techniques. In particular, information regarding the locations of substitutional ions present at low concentration was accessible (Mn and Rb in lepidolite--Evans & Raftery, 1982a; Ti and Na in biotite--Evans & Raftery, 1980aRaftery, , 1982b, and the direct quantitative determination of the aluminium distribution between tetrahedral and octahedral sites was demonstrated (Evans & Raftery, 1980b). It was suggested (Evans & Raftery, 1982a) that XPD might also be capable of characterizing cation ordering in micas--some of the data were only readily intelligible on the assumption that cation ordering could produce detectable effects in XPD--but much further work remained to be done.A far more comprehensive study of the same two micas using more sophisticated data collection techniques has now been completed; these new procedures are fully described elsewhere (Ash et al., 1987). In this paper only those aspects which relate to cation ordering in micas are discussed; XPD is now a powerful tool for the discovery and limited characterization of this phenomenon. The information accessible does not extend to bond lengths and angles, but, for example, differentiation of the three octahedral cation sites can now readily be made (as shown below). Moreover, although large crystals are still required, the degree of crystal perfection necessary is lower than for normal X-ray methods. EXPERIMENTALThe c-axis repeat distances were found by Cu-K~ oscillation photographs to be consistent with a single-layer repeat in both micas. Close approximations to a mirror plane were evident * Present address: English China

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“…To date, XPS has been applied to the study of the cations adsorbed on clay minerals (Koppelman and Dillard, 1975, 1978, 1980, the oxidation and reduction reactions of nontronite and biotite (Stucki et al, 1976;Stucki and Roth, 1977), the X-ray photoelectron diffraction (XPD) of single-crystal clay minerals (Adams et aL, 1978a(Adams et aL, , 1978bEvans and Raftery, 1979, 1980a, 1980b, 1982a, 1982b, the oxidation states of Ti and of Mn in clay minerals Raftery, 1980b, 1982c), calcined Co-kaolinite materials (Dillard et al, 1983), and the bonding state of the exchangeable divalent cations in montmorillonite (Seyama and Soma, 1984). In the present study, the effect of heating on the surface elemental composition and on the bonding state of the exchangeable cations in montmorillonite are reported on the basis of the XPS and XRD data.…”

Section: Introductionmentioning

confidence: 99%

X-Ray Photoelectron Spectroscopic Study of the Effect of Heating on Montmorillonite Containing Sodium and Potassium Cations

Seyama

1986

Clays and clay miner.

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Abstract-The effect of heating on montmorillonites containing exchangeable Na and K has been studied by X-ray photoelectron spectroscopy (XPS). The surface composition of the unheated montmorillonite was consistent with the bulk composition, but after the sample recrystallized at 1 100~ the surface abundance of Na increased, whereas that of K decreased. Because Na and K were not present in the hightemperature crystalline products, this behavior suggests that a noncrystalline material separated from the crystalline products. The Na 1 s binding energy and KL23L23 Auger kinetic energy ofmontmorillonite were comparable with those of Na in typically ionic compound, such as NaC1. These electron energies became smaller and larger, respectively, on heating and approached those of feldspar (albite). The K 2p3/2 binding energy of montmorillonite increased slightly on heating. The K 2p3/2 binding energy of heated sample of montmorillonite was also comparable with that of feldspar (orthoclase). These results suggest that Na and K were incorporated into feldspar-like noncrystalline materials.

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X-ray photoelectron studies of titanium in biotite and phlogopite

Cited by 15 publications

References 20 publications

X-ray photoelectron diffraction studies of lepidolite

X-ray photoelectron diffraction studies of lepidolite

Cation ordering in lepidolite and biotite studied by X-ray photoelectron diffraction

X-Ray Photoelectron Spectroscopic Study of the Effect of Heating on Montmorillonite Containing Sodium and Potassium Cations

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