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A high temperature structural phase transition in crocoite (PbCrO4) at 1068 K: crystal structure refinement at 1073 K and thermal expansion tensor determination at 1000 K

Published online by Cambridge University Press:  05 July 2018

K. S. Knight*
Affiliation:
ISIS Facility, CLRC Rutherford Appleton Laboratory, Chilton, Didcot, Oxfordshire, OX11 0QX, and Department of Mineralogy, Natural History Museum, Cromwell Road, London SW7 5BD, UK
*

Abstract

High-resolution, neutron time-of-flight, powder diffraction data have been collected on natural crocoite between 873 and 1073 K. Thermal analysis carried out in the 1920s had suggested that chemically pure PbCrO4 exhibited two structural phase transitions, at 964 K, to the β phase, and at 1056 K, to the γ phase. In this study, no evidence was found for the α-β structural phase transition, however a high-temperature phase transition was found at ∼1068 K from the ambient-temperature monazite structure type to the baryte structure type. The phase transition, close to the temperatures reported for the β to γ phase modifications, is first order and is accompanied by a change in volume of −1.6%. The crystal structure of this phase has been refined using the Rietveld method to agreement factors of Rp = 0.018, Rwp = 0.019, Rp = 0.011. No evidence for premonitory behaviour was found in the temperature dependence of the monoclinic lattice constants rom 873 K to 1063 K and these have been used to determine the thermal expansion tensor of crocoite just below the phase transition. At 1000 K the magnitudes of the tensor coefficients are α11, 2.66(1) × 10−5 K−1; α22, 2.04(1) × 10−5 K−1; α33, 4.67(4) × 10−5 K−1; and α13, −1.80(2) × 10−5 K−1 using the IRE convention for the orientation of the tensor basis. The orientation of the principal axes of the thermal expansion tensor are very close to those reported previously for the temperature range 50–300 K.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2000

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References

Brody, S.B. (1942) An X-ray investigation of the structure of lead chromate. J. Chem. Phys., 10, 650–2.CrossRefGoogle Scholar
Collotti, G., Conti, L. and Zocchi, M. (1959) The structure of the orthorhombic modification cation of lead chromate PbCrO4 . Acta Crystallogr., 12, 416.CrossRefGoogle Scholar
Ibberson, R.M., David, W.I.F. and Knight, K.S. (1992) The high resolution powder diffractometer (HRPD) at ISIS – a user guide. Rutherford Appleton Laboratory Report RAL-92-031.Google Scholar
Jaeger, F.M. and Germs, H.C. (1921) Über die binären systeme der sulfate, chromate, molybdate und wolframate des bleies. Zeit. Anorg. Chem., 119, 145–73.CrossRefGoogle Scholar
Jessen, S.M. and Küppers, H. (1991) The precision of thermal-expansion tensors of triclinic and monoclinic crystals. J. Appl. Crystallogr., 24, 239–42.CrossRefGoogle Scholar
Johnson, M.W. and David, W.I.F. (1985) HRPD: The high resolution powder diffractometer at the SNS. Rutherford Appleton Laboratory Report RAL-85- 112.Google Scholar
Knight, K.S. (1996) A neutron powder diffraction determination of the thermal expansion tensor of crocoite (PbCrO4) between 60 K and 290 K. Mineral. Mag., 60, 963–72.CrossRefGoogle Scholar
Náray-Szabó, I. And Argay, G. (1965) Die kristallstruktur des krokoites, PbCrO4 . Acta Chimica Acad. Scientiarum Hungarae, 40, 283–8.Google Scholar
Parkes, G.D. (1952) Mellor’s comprehensive treatise on inorganic and theoretical chemistry, volume 11, revised edition. Longmans, Green & Co.Google Scholar
Pawley, G.S. (1981) Unit cell refinement from powder diffraction scans. J. Appl. Cryst., 14, 357–61.CrossRefGoogle Scholar
Pistorius, C.W.F.T. and Pistorius, M.C. (1962) Lattice constants and thermal-expansion properties of the chromates and selenates of lead, strontium and barium. Zeits. Kristallogr., 117, 259–71.CrossRefGoogle Scholar
Popovkin, B.A. and Simanov, Yu.P. (1962) An X-ray diffraction study of the two modifications of lead selenate. Zh. Neorgan. Khim., 7, 1743–4.Google Scholar
Quareni, S. and De Pieri, R. (1964) La struttura della crocoite, PbCrO4 . Rend. Soc. Mineral. Italiana, 20, 253–250.Google Scholar
Quareni, S. and De Pieri, R. (1965) A three-dimensional refinement of the structure of crocoite, PbCrO4 . Acta Crystallogr., 19, 287–9.CrossRefGoogle Scholar
Quittner, F., Sagpir, J. and Rassudowa, N. (1932) Die rhombishe modi. kation des bleichromates. Zeit. Anorg. Chem., 204, 315–7.CrossRefGoogle Scholar
Schlenker, J.L., Gibbs, G.V. and Boisen, M.B. (1975) Thermal expansion coef. cients for monoclinic crystals: a phenomenological approach. Amer. Mineral., 60, 828–33.Google Scholar
Wagner, H. (1931) Optische und röntgenographische untersuchen an pigmenten. Zeit. Angew. Chem., 44, 665–7.CrossRefGoogle Scholar
Wagner, H., Haug, R. and Zipfel, M. (1932) Die modifikation des bleichromates. Zeit. Anorg. Chem., 208, 249–54.CrossRefGoogle Scholar