INVESTIGATION OF COMPRESSION AND THERMAL EXPANSION OF a-mnte USING A CUBIC-ANVIL X-RAY DIFFRACTION PRESS
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1 INVESTIGATION OF COMPRESSION AND THERMAL EXPANSION OF a-mnte USING A CUBIC-ANVIL X-RAY DIFFRACTION PRESS W.Paszkowicz, E.Dynowska and T.Peun* Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, 2-668, Warsaw, Poland *) GeoForschungsZentrum Potsdarn, Telegrafenberg A17, D Potsdam, Germany ABSTRACT Investigation of a-mnte was performed at high pressure-high temperature conditions at a synchrotron radiation X-ray source. The high pressures and temperatures were obtained with the help of a cubic anvil X-ray diffraction press, MAX8. Unit-cell parameters were determined at 296 K at pressures up to 67.5 kbar and at fixed pressure of 67.5 kbar in the temperature range from 296 to 1273 K. The obtained data allowed determination of the compressibility at 296 K and of the thermal expansion at 67.5 kbar. The calculated value of bulk modulus agrees with earlier reported data. INTRODUCTION Several high-temperature and high-pressure forms of MnTe have been reported [l- 4] (see Table 1): MnTe-I (or a-mnte), stable at ambient temperature and pressure, crystallizes in NiAs-type hexagonal structure. Two high-pressure phases are known [4]: MnTe-II of a structure related to NiAs type and orthorhombic MnTe-III of MnP structure type. Table 1 is completed by data of MnzTe3 and MnTe2 compounds. Discrepancies exist between different literature sources concerning the highpressure behaviour of a-mnte, in particular in the most recent paper the highpressure limit of occurrence of a-mnte has been found to be considerably lower (73 kbar 141) than that reported earlier (13 kbar [14]). The observed anomalies in the pressure variations of lattice-constants have been attributed to a magnetic transition [5]. There is one well known high-temperature form, P-MnTe, of NaCl structure type* The occurrence of other high-temperature forms, y and 6 of unknown structure types, reported in [2] seems to be not confirmed yet. Recently, thin MnTe films of sphalerite structure type were grown by molecular beam epitaxy ( see, e.g., [9] and references therein). The films exhibit interesting physical properties because of the presence of manganese atoms exhibiting magnetic moment in a typical semiconductor structure. EXPERIMENTAL The investigated MnTe sample was prepared by crystallization from vapour phase. Laboratory diffractometric measurements did not show any trace of secondary phases in it. The diffraction experiments were performed using synchrotron radiation at F2.1 bearnline at DESY-HASYLAB. The high pressure-high temperature conditions were obtained at a cubic anvil X-ray diffraction press, MAX8 (described, e.g., in [ 151). NaCl sample located in the close vicinity of the studied sample was used as a pressure marker while a thermocouple was used to determine the temperature. The estimated uncertainty in pressure was 1 kbar. The X-ray detection system was based on a germanium solid state detector of resolution 155 ev. Peak positions were obtained by profile fitting assuming the gaussian Copyright (C) shape. JCPDS-International The lattice Centre constants for Diffraction Data were 1997 calculated by least-squares method from ISSN 197-2, positions Advances of in nine X-ray Analysis, observed Volume peaks. 4 The compression was studied at 296 K in the r.. A- L hir.nr\n II I. I^
2 This document was presented at the Denver X-ray Conference (DXC) on Applications of X-ray Analysis. Sponsored by the International Centre for Diffraction Data (ICDD). This document is provided by ICDD in cooperation with the authors and presenters of the DXC for the express purpose of educating the scientific community. All copyrights for the document are retained by ICDD. Usage is restricted for the purposes of education and scientific research. DXC Website ICDD Website -
3 pressure range up to 67.5 kbar on uploading and the thermal expansion was studied at 67.5 kbar in the temperature range from 296 to 1273 K. Table 1. Reported compounds in the Mn-Te system. B, and B refer to the bulk modulus and its first pressure derivative, respectively. compound structure space lattice canstants B reference type group I4 & stability range MnTe-I (a-mnte) MnTe-II MnTe-III fmante NiAS? 4) NaCl y-mnte -9 &MnTe h4hte w P4hmc Pnma Fm3m sphalerite F-43m MnzTeJ a-crfe P4mnm MnTe2 Pyrite Pa-3 MnTez Pyrite Pa-3 MnTez marcasite Pnnm 4.151(9), 6.72(4) 4.158, , (l), 6.71 l(3) 6.119,5.773, , (l) 5.272(12), 6.144(12) 3.795(12) PI PI PI 1) [2] T < 1228 K thiswork 3) [4]p c 73 kbar 2) [4) 97 <p < 28 kbar [4] p >236 kba; [ cT<1293 K [7] D1312 IS 5) [2] 1293<T<1328 K [2] T> 1328 K [ii ; 8) c71 WI WI 9) [IlIp> 7ti5 kbar 1) calculated from compressibility cited in [12], 2) values jointly determined for both MnTe-I and MnTe-II forms, 3) data for P296 OK, 4) structure type probably related to NiAs type, 5) stable above 1312 OK or if grown from Te-rich melt, 6) structure of y and 6 phases has not been studied in [2], the authors have postulated the wurtzite and sphalerite type for them, respectively, believing that there may be an analogy with MnSe polymorphs, 7) data for thin films, 8) data derived by extrapolation from those of (Cd,Mn)Te given in [13] for thin films, Copyright (C) JCPDS-International 9) high-pressure Centre form Diffraction being a Data second 1997 MnTe2 form of pyrite type.
4 RESULTS AND DISCUSSION In the applied conditions, i.e. at 296 IS with pressure increasing up to 67.5 kbar, and with following temperature rise from 296 to 1273 K (at 67.5 kbar), the structure type of NiAs type is found to be conserved. Variations of the a-mnte unitcell constants with pressure on uploading up to 67.5 kbar are presented in Fig. 1. Compared to the previous high-pressure investigations [5,14], the experimental points obtained in this work are characterized by a much smaller scatter. This feature can be attributed to the favourable experimental conditions based on the setting of MAX8 facility at the synchrotron source (good statistics, precisely controlled temperature and pressure). With these conditions the lattice parameters could be calculated from nine peaks which gives a smaller error than if only two (as in [5]) or 4-6 (as in [14]) peaks are used, only. The results obtained do not confirm the anomalies of the lattice constant c dependence on pressure found in PI : a 6.65 z 6.6 U-J -J c 6.55 m PRESSURE [kbar] I I I I I I I i PRESSURE [kbar] Fig. 1. Variation of lattice constants of a-mnte as a function of pressure at 296 K. The compressibility dependence on pressure (Fig. 2) was used to determine the bulk modulus of the a-mnte phase. The bulk modulus and its first pressure derivative calculated by fitting the Birch-Murnaghan equation [ 161 are B,=473 kbar and db,/dp=3.. The B, value obtained in this work for a-mnte is slightly lower than the value 497 kbar obtained jointly for this phase and MnTe-II, and it is markedly lower than that of MnTe-III (B~584 kbar), both reported in [4]. This ISSN 197-2, sequence Advances of in values X-ray Analysis, in Volume agreement 4 with the expectation that high-pressure phases are stiffer than low-pressure phases, similarly to the properties of, e.g., MnTe:, [l l]
5 included in Table 1. Although the diffraction data of [4] are of a high accuracy, a full comparison with our work is not possible because the experimental points of the cited paper are located at higher pressures. z - (I) KJ w lx a 2 1.oo PRESSURE Fig. 2. Compressibility of a-mnte as a function of pressure at 296 K. The solid line refers to the fitted Birch-Mumaghan equation. [kbar] The dependence of unit-cell constants and volume with temperature at fixed 67.5 kbar pressure is shown in Fig. 3. It completes earlier investigations performed at ambient [17] and intermediate [5] pressures. The obtained dependences may be approximated by: a = T- 3.59*1-8 T2 (I) c = *1-4 T P (2) V= T e T2 (3) with temperature expressed in K, lattice constants in A and the cell volume in A3. The magnetic transition observed in a-mnte occurs just above room temperature and manifests itself by a strong (dc~o. 1 A) increase of the lattice constant c [ 171. Electrical resistivity measurements have shown [18] that the transition temperature increases with applied pressure. More detailed investigation would be needed to reveal this transition under high temperature-high pressure conditions applied in the present work. Copyright JCPDS-International Centre for Diffraction Data 1997
6 m,+ k 91- > I:/.,,, ( TEMPERATURE [K] 6.6 -) /A 6.45 I_. I I I TEMPERATURE [K] I I I I I I TEMPERATURE [K] Fig. 3 Unit-cell constants and volume of a-mnte at 67.5 kbar as a function of temperature. The solid lines corresponds to the approximations given by equations (l-3). Copyright JCPDS-International Centre for Diffraction Data 1997
7 ACKNOWLEDGEMENTS: The authors are indebted to Professor Andrzej Mycielski (Institute of Physics) for the MnTe sample. Partial support by Deutsche Forschungsgemainschaft is gratefully acknowledged. REFERENCES: 1. N.K.Abrikosov, K.A.Dyuldina, V.V.Zhdanova, Izv. Akad. Nauk USSR, Neorg. Mater. 4 (1968) V.G.Vanyarkho, V.P.Zlomanov, A.V.Novoselova, Izv. AN SSSR - Neorg. Mater. 6 (197) N.Kasai, Y.Nishihara and S.Ogawa, J.Phys. Sot. Jap. 51 (1982) M.Mimasaka, I.Sakamoto, K.Murata, Y.Fujii and A.Onodera, J.Phys. C: Solid State Phys. 2 (1987) H.Sugiura, A.Sawaoka, S.Saito and K.Inoue, J.Phys. Chem. Solids 4 (1979) ICDDO reference card No Landolt-Bdrnstein Numerical Data and Functional Relationships in Science and Technology, group III, vol.l4b, part 2 (Springer Verlag, Berlin 1986) p.217 J.R.Buschert, F.C.Peiris, N.Samarth, H.Luo and J.K.Furdyna, Phys. Rev. B49 (1994) E. Janik, E.Dynowska, J.Bqk-Misiuk, M.Leszczynski, W. Szuszkiewicz, T.Wojtowicz, G.Karczewski, AZakrzewski and J.Kossut, Thin Solid Films 267 (1995) H.FjellvAg, A.Kjekshus, T.Chattopadhyay, H.D.Hochheimer, W.Htjnle and H.G. von Schnering, Phys. Lett. 112A (1985) H.Fjellvbg, W.A.Grosshans, W.HGnle and A.Kjekshus, J.Magn. Magn. Mat. 145 (1995) A.M.Burkhanov, Ya.G.Smorodinsti and I.G.Fakidov, Fiz. Tver. Tela 18 (1976) P.Maheswarathan, K.J.Sladek and U.Debska, Phys. Rev. B31 (1985) H.Nagasaki, I.Wakabayashi and S.Minomura, J.Phys. Chem. Solids 3 (1969) B.Buras and L. Gerward, in: Progress in Crystal Growth and Characterizatation, vol. 18, ed. P.Krishna (Pergamon Press, Oxford 1989) pp R.M.Hazen and L.W.Finger, Comparative Crystal Chemistry, (John Wiley & Sons, Chichester 1982) H.P.Grazhdankina and D.P.Gurfel,.%x-n. Eksp. Teor. Fiz. 35 (1958) K.Ozawa, S.Anza.i and Y.Hamaguchi, Phys. Lett. 2 (1966)
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