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Article

Ternary Aluminides of a New Homologous Series—CePt2Al2 and CePt3Al3: Crystal Structures and Thermal Properties

by
Elena Murashova
*,
Yuliya Morozova
,
Sergey Dunaev
,
Zhanafiya Kurenbaeva
and
Anna Tursina
Department of Chemistry, Moscow State University, 119991 Moscow, Russia
*
Author to whom correspondence should be addressed.
Crystals 2020, 10(6), 465; https://doi.org/10.3390/cryst10060465
Submission received: 13 March 2020 / Revised: 21 May 2020 / Accepted: 22 May 2020 / Published: 1 June 2020
(This article belongs to the Special Issue Intermetallic)
Browse Figures
Versions Notes

Abstract

:
In the process of studying the Ce–Pt–Al system, we identified CePt2Al2 and CePt3Al3, two new ternary intermetallic compounds. CePt2Al2 aluminide undergoes a structural phase transition from a low-temperature orthorhombic modification (of its own structure type, Cmme, a = 5.84138(2) Å, b = 6.39099(3) Å, c = 10.11611(5) Å) to a high-temperature tetragonal modification (CaBe2Ge2 type, P4/nmm, a = 4.3637(9) Å, c = 10.0925(14) Å) at 280(1) °C. CePt3Al3 crystallizes with a new type of structure (Cmme, a = 6.36548(6) Å, b = 5.78301(6) Å, c = 13.36245(19) Å) built of structural units of low-temperature orthorhombic CePt2Al2-type and CsCl-type.

1. Introduction

The RET2X2 family (RE, rare earth element, actinoid, element of the 2nd group; T, transition metal; X, s- or p-block element) continues to attract attention from scientists due to their different physical properties related to strong electronic correlations such as heavy fermion states, superconductivity, valence fluctuations, unusual magnetic, and non-Fermi liquid behavior [1,2,3,4,5,6,7]. Most RET2X2 compounds crystallize in two structure types: CaBe2Ge2 (P4/nmm, a = 4.02(2) Å, c = 9.92(2) Å) [8] and ThCr2Si2 (I4/mmm, a = 4.043(1) Å, c = 10.577(2) Å) [9]. Both are ternary BaAl4-type derivatives [10]. In the BaAl4 structure type, Al atoms reside in two crystallographically different Wyckoff sites: 4d (0,1/2,1/4) and 4e (0,0,z). Those occupying 4d sites form two-dimensional square nets that are alternately capped above and below the plane by the atoms in 4e sites. Between the corrugated layers perpendicular to [001], Ba atoms are located.
The structure of ThCr2Si2 is an ordered version of BaAl4 with more than 1700 ternary intermetallics being known as isotypic. In the ThCr2Si2 type, 4d positions are filled by Cr, whereas those in 4e are occupied by Si atoms. Thus, the Cr atoms comprise the basal two-dimensional slab of square nets with Si atoms capping the nets in a “checkerboard” pattern. The corrugated [Cr2Si2] layers are inverted with respect to each other and are separated by Th atoms. The structure remains I-centered like the BaAl4 prototype.
In the structure of CaBe2Ge2, which is not as rich in ternary intermetallics, filling the square nets of the basal slab and the capping layers occurs in an alternating manner. If the basal slab in the first layer is formed by Be atoms with Ge capping the square nets, in the next layer, Ge atoms build the basal slab that is capped by Be atoms. Due to this architecture of staggered [Be2Ge2] layers, CaBe2Ge2 has a primitive unit cell. Remarkably, CaBe2Ge2 type intermetallics are more likely to demonstrate superconductivity at high temperatures [11].
Intermetallics with platinum—REPt2X2 most commonly crystallize in the CaBe2Ge2 type. Silicides REPt2Si2 (RE = Y, La−Nd, Sm, Gd–Lu, U, Th) crystallize in a CaBe2Ge2 type and do not undergo phase transition [12], although it has been previously reported [13,14] that they belong to the ThCr2Si2 type with statistical filling of 4d and 4e positions with Pt and Si atoms in space group I4/mmm. Platinum germanides REPt2Ge2 (RE = Ca, Y, La−Dy) demonstrate a monoclinic variant (P21) of tetragonal CaBe2Ge2 structure with parameters for LaPt2Ge2 a = 4.401 Å, b = 4.421 Å, c = 9.851 Å, and β = 90.50° [15]. Reinvestigation of the structure showed a doubling of one of the parameters: a = 9.953 Å, b = 4.439 Å, c = 8.879 Å, β = 90.62°, and P21/c. The monoclinic cell undergoes a phase transition to a tetragonal type CaBe2Ge2 when the temperature is increased [16]. No phase transitions were observed in the CePt2Sn2 stannide, which belongs to the CaBe2Ge2 type [17].
Several pnictides with a REPt2X2 composition (X = P, As, Sb) with RE = Eu, Ca, Sr, Ba [18,19] adopt a CaBe2Ge2 type. REPt2P2 compounds where RE = Ca, Eu crystallize in a new structure type, a variation of the CaBe2Ge2 structure with a doubled c parameter and space group I4/mmm. The structures of SrPt2Sb2, BaPt2As2, and EuPt2Sb2 pnictides belong to the CaBe2Ge2 type, while the SrPt2As2 and EuPt2As2 arsenides present an orthorhombic distortion (Pmmn) of its tetragonal cell. Both compounds exhibit polymorphism: the orthorhombic modification of EuPt2As2 transforms to a tetragonal type CaBe2Ge2 with increasing temperatures, while SrPt2As2 undergoes phase transition to a monoclinic (P21/c) cell when pressure is increased.
About half of the 30 known aluminides RET2Al2 demonstrate a structure similar to CaBe2Ge2 including T = Au, RE = La−Nd, Sm, Eu, Gd−Dy, Th, U, and Sr [20] as well as T = Pd, RE = La, Ce [21]. The two latter compounds exhibit structural instability at low temperatures [22].
Recently, a homologous series structurally related to the title compounds was described [23]. Cerium palladium aluminides with the general formula CePdnAln (n = 2–4) are built from CaBe2Ge2 and CsCl type structural fragments and crystallize in a tetragonal P4/nmm space group.
During our ongoing investigation of the Ce–Pt–Al phase diagram, two novel ternary aluminides were observed. Cerium platinum aluminum intermetallics CePt2Al2 and CePt3Al3 present a new homologous series CePtnAln with n = 2, 3, derived from the orthorhombic CePt2Al2 and distorted CsCl type. Preliminary data on the crystal structures of the orthorhombic CePt2Al2 and CePt3Al3 have been presented at conferences [24,25]. Herein, we report on two structural modifications of CePt2Al2, tetragonal and orthorhombic, the structural phase transition between them as well as the crystal structure of CePt3Al3 and peculiarities of the homologous series CePtnAln (n = 2, 3).

2. Materials and Methods

2.1. Synthesis

The synthesis of new compounds was performed using metallic cerium (99.98%), platinum (99.99%), and aluminum (99.999%) mixed in stoichiometric ratios by arc-melting in a pure argon atmosphere. In order to ensure homogenization, the alloys were overturned and melted several times. The ingot of CePt2Al2 was divided into six parts, sealed in evacuated quartz ampoules, and annealed at 250 °C, 320 °C, 550 °C, 650 °C, 700 °C, and 800 °C for 720 h. Afterward, the ampoules were rapidly quenched to room temperature using cold water. The alloy of CePt3Al3 was annealed in an evacuated ampoule at 700 °C for 720 h.

2.2. Energy Dispersive X-Ray Analysis

Energy dispersive X-ray (EDX) analysis of all annealed samples was performed using a Carl Zeiss LEO EVO 50XVP scanning electron microscope (SEM) with an EDX-spectrometer INCA Energy 450 (Oxford Instruments). The accelerating voltage was 20 kV. For quantitative microanalysis, the INCA energy dispersion microanalysis system contains predefined standards for all elements. Analysis accuracy can be improved by incorporating proprietary measured reference materials. CePtAl was used as an external standard. The samples under investigation were placed together with the standard in a hot pressing machine (Bühler), filled with an electrically conductive resin, and formed into a tablet. The surface of the tablet was sanded using sandpaper cloths of different grain sizes and then polished on a cloth with an Al2O3 paste. Finally, the tablet was washed for 5 min in an ultrasonic bath filled with ethanol. The uncertainty of measurements for each element did not exceed 0.7 at.%.

2.3. Powder X-Ray Diffraction

Powder X-ray diffraction (XRD) patterns for phase analysis and preliminary determination of unit cell parameters were obtained with a STOE STADI P transmission diffractometer (CuKα1-radiation (λ = 1.54056 Å), Ge(111)-monochromator, a linear position-sensitive detector, 3–5° ≤ 2θ ≤ 93–95°, step scan 0.01°, 10 s counting time per point), using a WinXpow program [26].

2.4. High Temperature Powder Synchrotron X-Ray Diffraction

A high-intensity, high-resolution X-ray source (λ = 0.399962(13) Å) at the European Synchrotron Radiation Facility (ESRF, Grenoble, France) was used in the temperature-dependent powder XRD experiments.
The powder of the sample was placed in an evacuated thin-walled quartz glass capillary with a diameter of 0.5 mm, which was rotated during measurements at a rate of 1200 rpm to improve the counting statistics. Calibration of the goniometer and refinement of the X-ray wavelength were performed using the Si NIST 640c silicon standard. Synchrotron XRD patterns were measured at an angle range of 2° ≤ 2θ ≤ 22.912° with a scan step of 0.002°.

2.5. Crystal Structure Determination

The crystal structures of the tetragonal and orthorhombic modifications of CePt2Al2 as well as CePt3Al3 were determined from experimental powder XRD data. Indexing of the powder XRD pattern was performed using TREOR and DICVOL programs implemented in WinXpow [26] and FULLPROFF [27,28] packages.
Tetragonal CePt2Al2. The preliminary parameters of tetragonal CePt2Al2 were established using a low-quality single crystal found as a single copy in a sample of stoichiometric composition heated to 1200 °C and quenched in ice-cold water, which allowed us to attribute the structure to the CaBe2Ge2 type.
The tetragonal unit cell parameters obtained from powder XRD (Table 1) were compatible with the structure types of ThCr2Si2 and CaBe2Ge2. Analysis of the systematic reflection conditions indicated a primitive unit cell, therefore the CaBe2Ge2 type was chosen as a structural model. For the Rietveld refinement of tetragonal CePt2Al2 with the MRIA program [29], a high-temperature powder XRD pattern collected at 350 °C was used. In the refinement, the observed anisotropic line broadening was approximated in the quartic form [30] with five variables in the case of tetragonal syngony. The result of the refinement is shown in Figure 1a and Table 1.
Orthorhombic CePt2Al2 and CePt3Al3. Careful examination of the systematic extinctions in the orthorhombic CePt2Al2 and CePt3Al3 datasets suggested a C-centered unit cell (h + k = 2n for all hkl), which prompted space groups Cmme, Cm2e, C2me, Cmm2, and C222. The best refinement results were obtained in the centrosymmetric space group Cmme. The structures of orthorhombic CePt2Al2 and CePt3Al3 were solved using the Patterson method with the SHELXS [31] program and sets of 115 and 162 reflection intensities, respectively, extracted from the powder XRD patterns after pseudo-Voigt fitting. The structures were refined via the Rietveld method using the FULLPROF program [27,28] for a single phase in the case of CePt2Al2 and for three phases in the case of CePt3Al3. For the latter, small impurities that had previously been detected by EDX (PtAl binary and orthorhombic CePt2Al2) were taken into account. The relevant crystallographic details for data collection and refinement are listed in Table 1; observed, calculated, and difference room-temperature XRD powder patterns are plotted in Figure 1b,c. The atomic coordinates and isotropic displacement parameters determined for tetragonal CePt2Al2, orthorhombic CePt2Al2, and CePt3Al3 are listed in Table 2, and selected interatomic distances are given in Table 3.

2.6. Differential Thermal Analysis

Thermal stability and temperature at which the structural phase transition of CePt2Al2 occurs were investigated by differential thermal analysis (DTA) at temperatures between 22 °C and 1200 °C, with a heating rate of 20° per minute in a stream of pure helium (sample mass ~20 mg) using a Netzsch STA449 F1 apparatus equipped with a Platinum RT analyzer.

3. Results and Discussion

3.1. Sample Characterization

Six samples of Ce20.0Pt40.0Al40.0 (at.%) annealed at 250 °C, 320 °C, 550 °C, 650 °C, 700 °C, and 800 °C for 720 h were investigated by powder XRD and EDX analyses. For all samples, the main phase had the Ce20.7Pt39.9Al39.4 (at.%) composition. The microstructure of the studied samples showed that the sample annealed at 800 °C was single-phase (Figure 2a), while those annealed at 250 °C, 320 °C, 550 °C, 650 °C, and 700 °C contained an additional unknown phase with a composition close to Ce23.9Pt50.7Al25.4 (at.%).
Microstructures of all samples are shown in Figure S1 in the Supplementary Materials. Microstructure of the Ce14.2Pt42.9Al42.9 (at.%) alloy annealed at 700 °C showed that, in addition, to the main Ce14.4Pt42.9Al42.7 (at.%) phase, the sample contained Pt50.2Al49.8 (at.%) and Ce20.0Pt40.4Al39.6 (at.%) as admixtures (Figure 2b).
According to powder XRD patterns, all samples of CePt2Al2 including the as-cast one, were single-phase and solely contained an orthorhombic modification of CePt2Al2 (Figure 1b, Figure S2a–g). As follows from the XRD pattern of CePt3Al3 after annealing, the sample contained PtAl and CePt2Al2 admixtures in the amount of 4 mass % and 9 mass %, respectively (Figure 1c).

3.2. Thermal Analysis and Temperature-Dependent XRD

Since two crystallographic modifications were identified for the CePt2Al2 compound, tetragonal and orthorhombic, additional studies of the phase transition of CePt2Al2 were conducted. DTA (22–1200 °C) was performed for a sample annealed at 550 °C. The heating curve showed a weak endothermic effect at 280(1) °C, which could be attributed to a structural transition from a low-temperature polymorph to a high-temperature one (Figure S3). The endothermal effect at 1100 °C corresponded to the melting point. Attempts to obtain a high-temperature polymorph of CePt2Al2 by thermal quenching in cold water failed.
To study the stability of the crystallographic phases of CePt2Al2 and their structural transformation, in situ temperature-dependent synchrotron X-ray diffraction measurements were performed. Figure 3a,b clearly demonstrates the changes in X-ray patterns that occurred between 250 and 300 °C.
XRD patterns observed within the range of 25–250 °C corresponded to the low-temperature orthorhombic modification, lt-CePt2Al2. However, a change was detected at 300 and 350 °C that indicates a transition to a tetragonal modification, ht-CePt2Al2. The second series of in situ X-ray experiments with the same sample within a temperature range of 220–320 °C with 10° incremental increases in temperature (Figure S4a,b) demonstrated a transition at 280 °C. These data strongly support the results observed with DTA measurements and together clearly demonstrate the temperature at which structural phase transition occurs, providing proof of its reversible nature. Further analyses of powder XRD patterns collected at 300 and 350 °C yielded the crystal structure of ht-CePt2Al2 (Figure 1a).

3.3. CePt2Al2 Crystal Structures

High-temperature modification of CePt2Al2 is a new representative of tetragonal CaBe2Ge2 type (space group P4/nmm, Pearson symbol tP10) with lattice parameters: a = 4.3637(9) Å, c = 10.0925(14) Å, and Z = 2 (Figure 1a). The lt-CePt2Al2 compound crystallizes with its own structure type (space group Cmme, Z = 4): a = 5.84138(2) Å, b = 6.39099(3) Å, c = 10.11611(5) Å (Figure 1b).
Though the general motif of the atomic arrangement in two polymorphs of CePt2Al2 seems very similar, some structure peculiarities can be pointed out.
ht-CePt2Al2. Following the CaBe2Ge2 type, ht-CePt2Al2 is constructed from two types of corrugated [Pt2Al2] layers perpendicular to [001], with cerium atoms situated between them (Figure 4a,b). In the Pt-based layer, interatomic distances Pt1–Al2 are equal to 2.420(7) Å, and in the Al-based layer, interatomic distances Pt2–Al1 are equal to 2.5544(15) Å, indicating significant chemical bonding in the layers. Neighboring [Pt2Al2] layers of two types are connected by Pt2–Al2 contacts that are slightly longer (2.672(17) Å).
lt-CePt2Al2. The orthorhombic modification lt-CePt2Al2 is a distorted variant of the high-temperature modification (Figure 4c,d). Symmetry reduction from tetragonal to orthorhombic involves differentiation of the lattice parameters alt and blt, which comprise diagonals a + b of the tetragonal unit cell of ht-CePt2Al2. Parameters alt and blt are related to those of the high-temperature polymorph as alt ≈ 2 aht and blt ≈ 2 aht with alt < blt. Parameter c remains relatively unchanged. The volume of the lt-CePt2Al2 unit cell is twice that of the ht-CePt2Al2 unit cell. The interatomic distances are similar to those observed in ht-CePt2Al2: Pt1–Al2 of 2.416(3) Å and Pt2–Al1 of 2.5313(6) Å within the layers, and Pt2–Al2 of 2.673(3) Å between the layers.
The Ce-centered polyhedra in both polymorphs can be described as hexagonal prisms of eight Pt and eight Al atoms with four additional atoms capping the side faces of the prisms. The range of Ce–Al and Ce–Pt bonding contacts are bigger in the structure of lt-CePt2Al2 compared to those in the ht-CePt2Al2 at 3.1727(7)–3.503(3) Å and 3.302(3)–3.402(7) Å, respectively. The platinum centered polyhedra can be regarded as a slightly distorted cuboctahedra (Pt1) and tetragonal antiprisms with one additional atom (Pt2). Aluminum atoms are located inside the distorted cuboctahedra (Al1) and mono-caped tetragonal antiprisms (Al2) (Table 3).

3.4. CePt2Al2 Phase Transition

The observed phase transition can be attributed to a second-order transition. The space group of lt-CePt2Al2 (Cmme) is a subgroup of ht-CePt2Al2 (P4/nmm). The main relationship in Bärnighausen formalism [32,33] is presented in Figure 5.
The phase transition is of a displacive nature. Both modifications have a common structural motif and the same local atomic environment. On heating lt-CePt2Al2, Pt and Al atoms slightly shift in the directions indicated by the arrows in Figure 6, which leads to the equalization of the Pt1–Pt1, Al1–Al1, Ce–Pt2, and Ce–Al2 interatomic distances and of parameters a and b, and consequently, to transition from an orthorhombic to a tetragonal unit cell (Figure 7a, Table 3). There is no appreciable volume reduction in phase transformation. The formula unit volume increases continuously when heating from 25 °C to 350 °C with a negligible jump at the transition temperature (Figure 7b).
A similar structural phase transition from the orthorhombic modification (Cmme) to the tetragonal modification (P4/nmm) for compounds with palladium—LaPd2Al2 and CePd2Al2—occurs at 91.5 (5) K and 13.5 (1) K, respectively [22]. Based on a comparison of cell dimensions, one can extrapolate that lt-CePt2Al2 is iso-structural with lt-CePd2Al2. The crystal structure of the latter compound was not determined. The difference between aorth and borth for lt-CePt2Al2 is equal to 0.55 Å, which is appreciably larger when compared to those for lt-LaPd2Al2 and lt-CePd2Al2 (0.12 Å and 0.14 Å, respectively).

3.5. CePt3Al3 Crystal Structure

The structure of CePt3Al3 reflects a distorted variant of the iso-stoichiometric CePd3Al3 compound [23] and crystallizes with its own type in the orthorhombic cell with dimensions a = 6.36548(6) Å, b = 5.78301(6) Å, c = 13.36245(19) Å, sp. gr. Cmme, Z = 4 (Figure 8a,b). Cell metrics of the CePt3Al3 and CePd3Al3 compounds correlate as follows: a(CePt3Al3) ≈ 2 a(CePd3Al3), b(CePt3Al3) ≈ 2 a(CePd3Al3), c(CePt3Al3) ≈ c(CePd3Al3), similar to the relationship between the metrics of lt-CePt2Al2 and ht-CePt2Al2. The group–subgroup relationship in Bärnighausen formalism [32,33] for the structures CePt3Al3 and CePd3Al3 is presented in Figure 8c. DTA of the CePt3Al3 sample did not demonstrate a thermal effect that indicated a possible phase transition.
Similar to lt-CePt2Al2, CePt3Al3 contains two types of two-dimensional [Pt2Al2] layers separated by Ce atoms. If the Al-based layer wholly complies with that of lt-CePt2Al2, two Pt-based layers are condensed to form a double layer in which capping Al atoms form the distorted squares of a planar network between two of those of Pt. The shortest Pt–Al interlayer distance Pt2–Al2 of 2.377(11) Å is significantly smaller than that of lt-CePt2Al2 and ht-CePt2Al2 (2.673 Å) and other Pt–Al contacts of CePt3Al3 of 2.5185(8)–2.640(7) Å (Table 3). A similarly short Pt–Al contact of 2.418(6) Å occurs in the Ce3Pt4Al6 structure [34].
In CePt3Al3, coordination polyhedra of Ce, Pt, and Al atoms largely resemble those observed in lt-CePt2Al2 and ht-CePt2Al2. In the environment of the Al2 atom, an additional Al3 neighbor of the double layer results in the formation of a double-capped tetragonal antiprism around the Al2 atom. The Al3 atom is surrounded by eight platinum atoms with Pt–Al separations ranging within 2.611(7)–2.640(7) Å in the form of a distorted CsCl-like cube. With the next-nearest five neighbors at distances up to 3.1831(3) Å away, a polyhedron derived from the cuboctahedron is formed.

3.6. New Homologous Series

The structures of lt-CePt2Al2 and CePt3Al3 can be presented as Ce-centered polyhedra, sharing common edges in the c-direction and common hexagonal faces perpendicular to the c-axis (Figure 8d). Alternating along the c-axis, similar adjacent layers are inverted and shifted relative to each other. In the CePt3Al3 structure, the double layer of Ce-polyhedra alternate with the [PtAl] layer of CsCl-like distorted cubes (Figure 8d). Ternary compounds of lt-CePt2Al2 and CePt3Al3 comprise a new homologous series built of structural units of lt-CePt2Al2 and CsCl-type: CePtnAln (n = 2, 3). Due to the addition of one [PtAl] layer with a thickness of 3.138 Å to the lt-CePt2Al2 structure, the c parameter of the unit cell expands from 10.11611(5) Å in lt-CePt2Al2 to 13.36245(19) Å in CePt3Al3. Homologous series of iso-stoichiometric palladium compounds [23] contains one more member (n = 4), which is composed of alternating double Ce-polyhedra and double [PdAl] layers. An iso-stoichiometric compound with platinum was not observed.

3.7. Crystal Structures of Cerium Platinum Aluminides with High Al Content

The crystal structures analyzed consist of three-dimensional networks of Pt and Al forming Ce-centered hexagonal prisms of alternating Pt and Al atoms at the vertices, which were also observed in the structures of cerium platinum aluminides with high Al content: CePtAl3 [35], CePt3Al5 [36], Ce4Pt9Al13 [37], and Ce2Pt9Al16 [38] (Figure 9). In these structures, one of the unit cell parameters is about 4.2 Å, which corresponds to the height of the Ce-hexagonal prism. In the structures of ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3 as well as in CePtAl3, there are two-dimensional layers of condensed Ce-centered hexagonal prisms, in contrast to the infinite isolated single channels of hexagonal prisms in CePt3Al5 and Ce2Pt9Al16, and combinations of single and condensed triple channels of hexagonal prisms in the Ce4Pt9Al13 compound (Figure 9).

4. Conclusions

Cerium platinum aluminides were synthesized. DTA and in situ temperature-dependent synchrotron X-ray diffraction measurements showed a reversible phase transition from a low-temperature orthorhombic CePt2Al2 of its own type to a high-temperature tetragonal CePt2Al2 of a CaBe2Ge2 type when heated to a temperature above 280 °C. The phase transition is of a displacive nature and associated with slight distortions of the [Pt2Al2] layers. Orthorhombic compounds CePt2Al2 and CePt3Al3 present a new homologous series CePtnAln (n = 2, 3) formed from fragments of lt-CePt2Al2 and CsCl types.

Supplementary Materials

The following are available online at https://www.mdpi.com/2073-4352/10/6/465/s1, Figure S1: The microstructure of the Ce20.0Pt40.0Al40.0 (at.%) samples annealed at 250 °C, 320 °C, 550 °C, 650 °C, and 700 °C; Figure S2(a–h): XRD patterns of Ce20.0Pt40.0Al40.0 (at.%) samples; Figure S3: DTA heating thermogram of the CePt2Al2 sample; Figure S4: (a,b) Structural transition of low-temperature orthorhombic CePt2Al2 to a high-temperature tetragonal modification. XRD patterns at 220, 230, 240, 250, 260, 270, 280, 290, 300, 310, 320 °C (a); a projection of XRD patterns (b).

Author Contributions

Conceptualization, E.M. and Y.M.; Methodology, E.M. and A.T.; Formal analysis, Y.M. and Z.K.; Investigation, E.M., Y.M., Z.K., and A.T.; Resources, E.M.; Writing—original draft preparation, E.M.; Writing—review and editing, A.T.; Visualization, Y.M.; Supervision, E.M. and S.D.; Project administration, E.M.; Funding acquisition, E.M. All authors have read and agreed to the published version of the manuscript.

Funding

This study was supported by the Russian Foundation for Basic Researches (Grant No. 19-03-00135a).

Acknowledgments

The experimental data for the X-ray structure analysis were obtained using equipment at the Shared Physical Characterization Facilities Center, Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences. The authors are indebted to ESRF-Grenoble for providing access to the ID22 Station (experiment MA-3313).

Conflicts of Interest

The authors have no conflicts of interest to declare. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in manuscript composition, or in the decision to publish the results.

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Crystals 10 00465 g001a 550Crystals 10 00465 g001b 550
Figure 1. Observed (red dots), calculated (black solid line), and difference (bottom blue line) powder X-ray diffraction (XRD) patterns for tetragonal CePt2Al2 (a), orthorhombic CePt2Al2 (b), and CePt3Al3 (c).
Figure 1. Observed (red dots), calculated (black solid line), and difference (bottom blue line) powder X-ray diffraction (XRD) patterns for tetragonal CePt2Al2 (a), orthorhombic CePt2Al2 (b), and CePt3Al3 (c).
Crystals 10 00465 g001aCrystals 10 00465 g001b
Crystals 10 00465 g002 550
Figure 2. Microstructure of the Ce20.0Pt40.0Al40.0 (at.%) alloy annealed at 800 °C (a) and of the Ce14.2Pt42.9Al42.9 (at.%) alloy annealed at 700 °C (b) obtained using scanning electron microscopy (SEM).
Figure 2. Microstructure of the Ce20.0Pt40.0Al40.0 (at.%) alloy annealed at 800 °C (a) and of the Ce14.2Pt42.9Al42.9 (at.%) alloy annealed at 700 °C (b) obtained using scanning electron microscopy (SEM).
Crystals 10 00465 g002
Crystals 10 00465 g003 550
Figure 3. Structural transition of the low-temperature orthorhombic CePt2Al2 to the high-temperature tetragonal modification. (a) XRD patterns measured at 25, 100, 150, 200, 250, 300, and 350 °C; (b) a projection of XRD patterns.
Figure 3. Structural transition of the low-temperature orthorhombic CePt2Al2 to the high-temperature tetragonal modification. (a) XRD patterns measured at 25, 100, 150, 200, 250, 300, and 350 °C; (b) a projection of XRD patterns.
Crystals 10 00465 g003
Crystals 10 00465 g004 550
Figure 4. Crystal structures of two CePt2Al2 modifications: projection of ht-CePt2Al2 along the b-axis (a), projection of lt-CePt2Al2 in [110] (c), projections along the c-axis of the Pt-based layer of ht-CePt2Al2 (b), and of lt-CePt2Al2 (d). The Al2 atoms positioned above two-dimensional Pt-based basal layer are pink and those positioned below are rose. Unit cells are outlined in red.
Figure 4. Crystal structures of two CePt2Al2 modifications: projection of ht-CePt2Al2 along the b-axis (a), projection of lt-CePt2Al2 in [110] (c), projections along the c-axis of the Pt-based layer of ht-CePt2Al2 (b), and of lt-CePt2Al2 (d). The Al2 atoms positioned above two-dimensional Pt-based basal layer are pink and those positioned below are rose. Unit cells are outlined in red.
Crystals 10 00465 g004
Crystals 10 00465 g005 550
Figure 5. Group–subgroup scheme in the Bärnighausen formalism for the structures of ht-CePt2Al2 and lt-CePt2Al2.
Figure 5. Group–subgroup scheme in the Bärnighausen formalism for the structures of ht-CePt2Al2 and lt-CePt2Al2.
Crystals 10 00465 g005
Crystals 10 00465 g006 550
Figure 6. Projection of the crystal structure of lt-CePt2Al2 onto the (001) plane. The arrows indicate the direction of atomic displacements that lead to the transition to the tetragonal ht-CePt2Al2 modification. The orthorhombic unit cell is outlined in red, and the tetragonal cell with a black dashed line.
Figure 6. Projection of the crystal structure of lt-CePt2Al2 onto the (001) plane. The arrows indicate the direction of atomic displacements that lead to the transition to the tetragonal ht-CePt2Al2 modification. The orthorhombic unit cell is outlined in red, and the tetragonal cell with a black dashed line.
Crystals 10 00465 g006
Crystals 10 00465 g007 550
Figure 7. Temperature-dependent evolution of the unit cell dimensions in CePt2Al2 (a) and of the scaled unit cell volume V/Z (Z is the formula unit per unit cell) (b). The error bars are smaller than the size of the plotted symbols and range from 0.0002 to 0.003 Å for parameters and from 0.3 to 0.6 Å3 for scaled unit cell volumes.
Figure 7. Temperature-dependent evolution of the unit cell dimensions in CePt2Al2 (a) and of the scaled unit cell volume V/Z (Z is the formula unit per unit cell) (b). The error bars are smaller than the size of the plotted symbols and range from 0.0002 to 0.003 Å for parameters and from 0.3 to 0.6 Å3 for scaled unit cell volumes.
Crystals 10 00465 g007
Crystals 10 00465 g008 550
Figure 8. Crystal structure of CePt3Al3, with projection in [110] (a) and projection along the c-axis (b). Unit cells are outlined in red. Group–subgroup relations in the structures of CePt3Al3 and CePd3Al3 (c). Homologous series of CePtnAln (n = 2, 3) (d).
Figure 8. Crystal structure of CePt3Al3, with projection in [110] (a) and projection along the c-axis (b). Unit cells are outlined in red. Group–subgroup relations in the structures of CePt3Al3 and CePd3Al3 (c). Homologous series of CePtnAln (n = 2, 3) (d).
Crystals 10 00465 g008
Crystals 10 00465 g009 550
Figure 9. Projections of networks of crystal structures of ht-CePt2Al2, CePtAl3, Ce4Pt9Al13, CePt3Al5, and Ce2Pt9Al16 in a direction along the smallest unit cell parameter and along [110] for lt-CePt2Al2 and CePt3Al3 structures. Ce, Pt, and Al atoms are drawn as green, black, and rose spheres, respectively. Single and triple Ce-atom channels and 2D Ce-atoms layers are highlighted in yellow.
Figure 9. Projections of networks of crystal structures of ht-CePt2Al2, CePtAl3, Ce4Pt9Al13, CePt3Al5, and Ce2Pt9Al16 in a direction along the smallest unit cell parameter and along [110] for lt-CePt2Al2 and CePt3Al3 structures. Ce, Pt, and Al atoms are drawn as green, black, and rose spheres, respectively. Single and triple Ce-atom channels and 2D Ce-atoms layers are highlighted in yellow.
Crystals 10 00465 g009
Table
Table 1. Crystal data and structural refinement for the ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3 compounds.
Table 1. Crystal data and structural refinement for the ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3 compounds.
Empirical Formulaht-CePt2Al2lt-CePt2Al2CePt3Al3 *
Molar mass, g/mol584.26584.26806.33
Structure type, Pearson symbolCaBe2Ge2, tP10CePt2Al2, oC20CePt3Al3, oC28
Space group, ZP4/nmm (129), 2Cmme (67), 4Cmme (67), 4
Unit cell dimensions
a, Å4.3637(9)5.84138(2)6.36548(6)
b, Å4.3637(9)6.39099 (3),5.78301(6)
c, Å10.0925(14)10.11611(5)13.36245(19)
V, Å3
Calculated density, g/cm3		192.18(6)
10.097		377.657
(3)10.276		491.894(10)
10.888
T, K623(1)295(1)298(2)
Radiation, λ, Åsynchrotron, 0.399962(13)CuKα1, 1.54056CuKα1, 1.54056
2θ range, step°2–22.912, 0.0025–95.19, 0.013–93.09, 0.01
Total no. reflections79115162
Refined parameters no.351229
Rietveld reliability factors
Rp0.0600.0240.037
Rwp0.0690.0350.050
Rexp0.0600.0160.020
χ21.3345.545.99
* All indicators—R-factors, no. of parameters, etc. are given for the three-phases refinement.
Table
Table 2. Atomic coordinates and isotropic displacement parameters in the crystal structures of ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3.
Table 2. Atomic coordinates and isotropic displacement parameters in the crystal structures of ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3.
AtomMultiplicity,
Wyckoff Letter,
Site Symmetry		x/ay/bz/cUiso., Å2
ht-CePt2Al2
Ce12c(4mm)1/41/40.7456(3)0.0211(9)
Pt12b(-4m2)3/41/41/20.0211(9)
Pt22c(4mm)1/41/40.1316(3)0.0211(9)
Al12a(-4m2)3/41/400.0211(9)
Al22c(4mm)1/41/40.3963(17)0.0211(9)
lt-CePt2Al2
Ce14g(mm2)01/40.24780(15)0.0117(4)
Pt14a(222)1/41/200.0224(4)
Pt24g(mm2)01/40.62972(11)0.0146(3)
Al14b(222)1/41/21/20.019(2)
Al24g(mm2)01/40.8940(7)0.013(2)
CePt3Al3
Ce14g(mm2)01/40.30545(16)0.0097(7)
Pt18l(…2)1/41/20.11280(8)0.0046(4)
Pt24g(mm2)01/40.59815(12)0.0064(5)
Al14b(222)1/41/21/20.001(3)
Al24g(mm2)01/40.7760(8)0.039(5)
Al34g(mm2)01/4−0.0019(9)0.057(5)
Table
Table 3. Selected interatomic distances (d) in ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3 structures.
Table 3. Selected interatomic distances (d) in ht-CePt2Al2, lt-CePt2Al2, and CePt3Al3 structures.
ht-CePt2Al2lt-CePt2Al2CePt3Al3
Atom 1Atom 2d, ÅAtom 1Atom 2d, ÅAtom 1Atom 2d, Å
Ce14Pt13.302(3)Ce14Pt13.3120(11)Ce14Pt13.3540(18)
4Pt23.3251(18) 2Pt23.1727(7) 2Pt23.1655(11)
4Al13.369(3) 2Pt23.4273(7) 2Pt23.4335(10)
4Al23.402(7) 4Al13.3458(12) 4Al13.3736(16)
2Al23.254(3) 2Al23.090(4)
2Al23.503(3) 2Al23.364(4)
Pt14Al22.420(7)Pt14Al22.416(3)Pt12Al32.611(7)
4Pt13.0856(6) 2Pt12.9207(10) 2Al22.614(6)
4Ce13.302(3) 2Pt13.1955(15) 2Al32.640(7)
4Ce3.3120(11) 2Pt12.8915(13)
Pt13.0146(15)
2Pt13.1827(13)
2Ce13.3540(18)
Pt24Al12.5544(15)Pt24Al12.5313(6)Pt2Al22.377(11)
Al22.672(17) Al22.673(7) 4Al12.5185(8)
4Ce13.3251(18) 2Ce13.1727(7) 2Ce13.1655(11)
2Ce13.4273(7) 2Ce13.4335(10)
Al14Pt22.5544(15)Al14Pt22.5313(6)Al14Pt22.5185(8)
4Al13.0856(6) 2Al12.9207(10) 2Al12.8915(13)
4Ce13.369(3) 2Al13.1955(15) 2Al13.1827(13)
4Ce13.3458(12) 4Ce3.3736(16)
Al24Pt12.420(7)Al24Pt12.416(3)Al2Pt22.377(11)
Pt22.672(17) Pt22.673(7) 4Pt12.614(6)
4Ce13.402(7) 2Ce13.254(3) Al32.968(16)
2Ce13.503(3) 2Ce13.090(4)
2Ce13.364(4)
Al34Pt12.611(7)
4Pt12.640(7)
2Al32.8920(3)
Al22.968(16)
2Al33.1831(3)
Further details regarding the investigation of the crystal structures may be obtained from CCDC/FIZ: CSD-1988138 (tetragonal CePt2Al2), CSD-1988139 (orthorhombic CePt2Al2), and CSD-1988140 (CePt3Al3).

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Murashova, E.; Morozova, Y.; Dunaev, S.; Kurenbaeva, Z.; Tursina, A. Ternary Aluminides of a New Homologous Series—CePt2Al2 and CePt3Al3: Crystal Structures and Thermal Properties. Crystals 2020, 10, 465. https://doi.org/10.3390/cryst10060465

AMA Style

Murashova E, Morozova Y, Dunaev S, Kurenbaeva Z, Tursina A. Ternary Aluminides of a New Homologous Series—CePt2Al2 and CePt3Al3: Crystal Structures and Thermal Properties. Crystals. 2020; 10(6):465. https://doi.org/10.3390/cryst10060465

Chicago/Turabian Style

Murashova, Elena, Yuliya Morozova, Sergey Dunaev, Zhanafiya Kurenbaeva, and Anna Tursina. 2020. "Ternary Aluminides of a New Homologous Series—CePt2Al2 and CePt3Al3: Crystal Structures and Thermal Properties" Crystals 10, no. 6: 465. https://doi.org/10.3390/cryst10060465

APA Style

Murashova, E., Morozova, Y., Dunaev, S., Kurenbaeva, Z., & Tursina, A. (2020). Ternary Aluminides of a New Homologous Series—CePt2Al2 and CePt3Al3: Crystal Structures and Thermal Properties. Crystals, 10(6), 465. https://doi.org/10.3390/cryst10060465

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