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Journal of Thermal Analysis and Calorimetry

, Volume 133, Issue 3, pp 1589–1596 | Cite as

Thermodynamic properties of the NdBr3–MBr binary systems (M = Na, K)

  • Yassine Bounouri
  • Madjid Berkani
  • Abdelmalek Zamouche
  • Anna Dańczak
  • Ida Chojnacka
  • Leszek Rycerz
Open Access
Article
  • 260 Downloads

Abstract

Phase equilibria in the NdBr3–MBr binary systems (M = Na, K) were established by differential scanning calorimetry. The system with NaBr is a simple eutectic system with two compounds that decompose in the solid state (NaNdBr4 at 603 K and Na3NdBr6 at 580 K). In the system with KBr, three stoichiometric compounds exist. First (K3NdBr6) is formed from KBr and K2NdBr5 at 680 K and melts congruently at 918 K. Second (KNd2Br7) melts congruently at 814 K. Third compound (K2NdBr5) melts incongruently at 822 K.

Keywords

Phase diagrams Phase transitions Thermal analysis Enthalpy DSC 

Introduction

Lanthanide bromides and iodides have been used in various technological applications. They are attractive components for doses in high-intensity discharge lamps and new highly efficient light sources with energy-saving features [1, 2, 3, 4, 5, 6, 7, 8, 9]. When they are combined with other metal halides, they can be applied in designing light sources with high efficacy and good color rendition. Photoluminescence and photo-stimulated luminescence of lanthanide-doped bromide materials have made research targeted at commercial X-ray storage phosphors [10] more intense lately, while laser activity in lanthanide-doped bromide host crystals has been achieved recently [11, 12, 13]. The scintillation properties of lanthanide halides determine their application as highly sensitive radiation detectors [14, 15]. As it was pointed out in a recent review [16], the properties of many rare-earth halides are poorly characterized and the bromides have received even less attention than chlorides and iodides. However, the rare-earth bromides importance is certainly not reflected in the amount of available experimental information on the thermodynamic characterization of both condensed and vapor phases. Only a few works concerning phase diagrams of LnBr3–MBr binary systems (Ln = lanthanide, M = alkali metal) have been reported in the literature [17, 18, 19, 20, 21]. The phase diagrams were presented in a graphic form only, without numerical data. In addition, significant discrepancies can be found between the data reported by different authors. For example, Vogel [17] claims an existence of only two compounds (Cs3SmBr6 and CsSm2Br7) in the SmBr3–CsBr system, whereas according to Blachnik and Jaeger-Kasper’s investigation [18] four compounds (Cs3SmBr6, Cs3Sm2Br9, Cs2SmBr5 and CsSm2Br7) are present in this system. The phase diagram of TmBr3–RbBr given by Molodkin et al. is very doubtful [21], which, contrary to all the other lanthanide bromide–rubidium bromide systems, was found to be a simple eutectic system. Another example of discrepancies is the LaBr3–CsBr binary phase diagram. According to Vogel [17], two compounds (Cs3LaBr6 and CsLa4Br13) exist in it, whereas investigation of Seifert and Yuan [22] performed later by DTA method showed an existence of three compounds (Cs3LaBr6, Cs2LaBr5 and CsLa2Br7), only one of which had the same stoichiometry as the one reported in the older work [17]. The same discrepancies concern the NdBr3–KBr system. According to Blachnik and Jaeger-Kasper [18], three compounds (K3NdBr6, K3NdBr6, K2NdBr5 and KNd2Br7 and KNd2Br7) are present in this system. Two of them melt congruently (K3NdBr6 and KNd2Br7), and third (K2NdBr5) melts incongruently. However, later literature data [23] are completely different. They suggest an existence of only two compounds (KNd2Br7 and K3NdBr6). In addition, their behavior is completely different. First of them decomposes in the solid state, and second melts incongruently. Therefore, we decided to reinvestigate this system in order to clarify the situation. In addition, we have investigated also phase equilibria in the NdBr3–NaBr binary system. These investigations are part of our general research program targeted at determination of unknown and verification of existing phase diagrams of lanthanide halide–alkali metal halide systems. Previously, we reported the results of investigations concerning the phase diagrams of the CeBr3–MBr (M = alkali metal) [24, 25, 26, 27, 28], PrBr3–MBr [29, 30, 31, 32], TbBr3–MBr [33, 34, 35] and DyBr3–MBr [36, 37, 38, 39] binary systems. The present paper is a continuation of this ongoing extensive program. It presents the phase equilibria in the NdBr3–MBr (M = Na, K) binaries. Some preliminary results concerning NdBr3–KBr system were presented during the conference [40]; however, they were never published.

Experimental

Chemicals and samples preparation

Neodymium(III) bromide used in the investigation was prepared by the so-called wet method [39] from the neodymium(III) oxide (Sigma-Aldrich, min. 99.9%). The main steps of this synthesis included dissolution of neodymium oxide in hot concentrated hydrobromic acid (Fluka > 48%), crystallization of hydrated neodymium bromide, dehydration and melting of anhydrous bromide in the presence of excess ammonium bromide as well as purification of neodymium bromide by distillation under reduced pressure (10−5 Pa) in a quartz ampoule at 1150 K. NdBr3 prepared in this way was of high purity (minimum 99.9%). Chemical analysis was performed by complexometric (neodymium) and mercurimetric (bromine) methods. The results were as follows: Nd, 37.55 ± 0.15% (37.57% theoretical), and Br, 62.45 ± 0.11% (62.43% theoretical).

Alkali metal bromides (NaBr and KBr) were Merck Suprapur reagents (minimum 99.9%). Before use, they were progressively heated up to fusion under gaseous HBr atmosphere. Excess of HBr was then removed from the melt by argon bubbling. All chemicals were handled inside a high-purity argon atmosphere in a glove box (water content < 2 ppm).

The NdBr3 and KBr or NaBr mixtures (in appropriate proportions weighed with precision of about 1 mg) were prepared in vacuum-sealed quartz ampoules and melted in electric furnace at 1150 K. After homogenization and solidification, these samples were ground in an agate mortar in a glove box. Different compositions prepared in this way were used both in phase diagram and in electrical conductivity measurements.

Measurements

Phase equilibria in the NdBr3–MBr (M = Na, K) systems were investigated with a Setaram LABSYS evo 1600 differential scanning calorimeter. Experimental samples (200–500 mg) were stored in vacuum-sealed quartz ampoules. Experiments were conducted at heating and cooling rates of 5 K min−1. Prior to measurements, the apparatus was calibrated by measurements of temperatures and enthalpies of phase transitions of standard substances [In, Sn, Zn, Sb and Ag metals of high purity (99.999%)]. The results obtained were used in calculation of temperature and enthalpy correction coefficients, which were introduced into apparatus software. Subsequently, apparatus was tested with high-purity metals and results obtained showed that the maximum relative experimental error on enthalpy of phase transition did not exceed 1%. Temperature was measured with precision ± 1 K.

Results and discussion

NdBr3–NaBr phase diagram

DSC investigations, performed on 21 samples with different compositions with heating and cooling rates of 5 K min−1, yielded both the corresponding temperature and enthalpy values. Due to a supercooling effect, all the experimental temperature and enthalpy values reported in this work were determined from heating curves. In all heating runs, the maximum at the highest temperature corresponds to the liquidus temperature; in all the other cases, onset temperature (Tons) was assumed as the effect temperature. The analysis of the DSC curves was performed with Setaram Calisto software, which also allowed us to separate overlapping peaks.

Some characteristic DSC heating curves are presented in Fig. 1. In the whole composition range, three endothermic peaks were present in all the heating curves. The effect at the highest temperature corresponds, as stated previously, to the liquidus temperature. The second peak also observed in all the samples at 645 K (a mean value from all the samples) can be related to the NaBr–NdBr3 eutectic. The eutectic contribution to the enthalpy of fusion was determined, and it is plotted versus composition in Fig. 2c. This so-called Tammann construction makes it possible to accurately estimate the eutectic composition from the intercept of the two linear parts in Fig. 2c, as x (NdBr3) = 0.443. The mixture with eutectic composition melts with enthalpy ΔfusHm = 14.9 kJ mol−1.
Fig. 1

DSC heating curves for NaBr–NdBr3 mixtures of different compositions: a x NdBr3 = 0.751, b x NdBr3 = 0.950, c x NdBr3 = 0.050, d x = 0.100

Fig. 2

Tammann diagram of NdBr3–NaBr binary system: a decomposition of Na3NdBr6 compound; b decomposition of NaNdBr4 compound; c NdBr3–NaBr eutectic composition

The third effect, at 603 K (a mean value from the measurements), is also observable in all the curves. The Tammann diagram was constructed for this effect (Fig. 2b). The intercept of the two linear parts in this diagram takes place at x(NdBr3) = 0.485, thus suggesting the existence of a compound with stoichiometry NaNdBr4. This compound decomposes in the solid state with enthalpy of 8.4 kJ mol−1.

In the composition range 0 < x ≤ 0.500, where x is a mole fraction of NdBr3, an additional effect at about 580 K was observed on the DSC curves (Fig. 1c, d). The Tammann diagram for this effect gives value x(NdBr3) = 0.236, which corresponds to the stoichiometry Na3NdBr6 quite well. Accordingly, this effect can be ascribed to decomposition of Na3NdBr6 in the solid state.

All the experimental results are listed in Table 1, and the phase diagram is shown in Fig. 3.
Table 1

Results of the DSC experiments performed for the NdBr3–NaBr binary system: T1—decomposition of Na3NdBr6 in the solid state, T2—decomposition of NaNdBr4 in the solid state, T3—temperature of NaBr–NdBr3 eutectic

X(NdBr3)

T1/K

T2/K

T3/K

TLiq/K

0.000

1022

0.050

580

599

636

994

0.100

581

603

654

964

0.150

582

604

641

917

0.200

580

605

640

856

0.250

582

606

635

818

0.300

579

605

651

732

0.350

580

606

646

696

0.400

580

606

638

0.450

580

605

645

681

0.500

602

646

732

0.551

602

645

774

0.600

602

643

812

0.650

602

642

806

0.700

601

645

859

0.751

599

643

879

0.798

605

643

903

0.849

602

661

917

0.900

602

640

938

0.950

602

637

949

1.000

954

Fig. 3

Phase diagram of the NdBr3–NaBr system

A graphic form of the phase diagram reported by Vogel [17] was the only experimental literature information about this system. According to this information, the system under investigation is an eutectic system with an additional effect taking place in the solid phase at 591 K. The nature of this effect was not explained by author. Our finding for the eutectic composition agrees with the literature information quite well (x = of about 0.436, as estimated from the graphic form of the phase diagram), whereas our eutectic temperature is lower by 7 K. The effect in the solid phase was observed by us at temperature 603 K, and it was ascribed to decomposition of NaNdBr4 compound into NaBr and NdBr3 in the solid state. This compound has a completely different stoichiometry from that assumed in the literature [41], where it was defined as either Na3NdBr6 or Na2NdBr5. Additional thermal effect at 580 K, observed for the first time by us, was not reported in the literature. We could ascribe it to the Na3NdBr6 compound, which decomposes in the solid state into NaNdBr4 and NaBr.

NdBr3–KBr phase diagram

DSC investigations were performed for 28 samples with different compositions covering the entire composition range. The temperature and the fusion enthalpy of the related mixtures were obtained from the corresponding heating curves. Some characteristic DSC heating curves are presented in Fig. 4. The effects at the highest temperature are undoubtedly related to the liquidus temperatures. In the composition range 0 < x < 0.250, where x is NdBr3 mol fraction, two additional endothermic peaks were present in addition to the liquidus effect (Fig. 4a). The first one, observed in all the samples up to x  = 0.250 at 849 K, can be undoubtedly ascribed to the KBr–K3NdBr6 eutectic. The eutectic composition, x (NdBr3) = 0.192, was determined accurately from the Tammann plot presented in Fig. 5a, and the enthalpy of fusion at the eutectic composition is ΔfusHm = 13.6 kJ mol−1. The second thermal effect, at 680 K (mean value from the measurements), was observable in all the curves up to x = 0.333, the composition at which it disappeared. This thermal effect corresponds to the formation of K3NdBr6 compound from MX and M2LnX5. The molar enthalpy related to this effect [calculated for K3NdBr6 compound (Fig. 5b)], ΔformHm = 45.8 kJ mol−1, is in a good agreement with the enthalpy observed for the formation of many M3LnX6 compounds (M = alkali metal, Ln = lanthanide, X = halide) [42]. For the mixture with x = 0.250, only peaks at 683 and 918 K were observed in the curve (Fig. 4b). The latter peak has a typical shape of a congruently melting compound. We deduced that congruently melting K3NdBr6 compound exists in the NdBr3–KBr system.
Fig. 4

DSC heating curves for KBr–NdBr3 mixtures of different compositions: a x NdBr3 = 0.051, b x NdBr3 = 0.250, c x NdBr3 = 0.270, d x NdBr3 = 0.595, e x NdBr3 = 0.850

Fig. 5

Tammann diagram of NdBr3–KBr binary system: determination of: a KBr–K3NdBr6 eutectic, b K3NdBr6 formation, c K2NdBr5 incongruent melting, d K2NdBr5–KNd2Br7 eutectic, e KNd2Br7–NdBr3 eutectic

In the composition range 0.250 < x < 0.333, two endothermic peaks were also present in addition to the liquidus effect (Fig. 4c). The first effect at 680 K (a mean value) agrees very well with effect observed for samples with molar fraction of NdBr3 0 < x < 0.250 and is undoubtedly related to formation of K3NdBr6 compound. Its disappearance at x = 0.333 suggests an existence of another compound, namely K2NdBr5. The second effect occurs at about 822 K in all the curves up to x = 0.400, the composition at which it disappeared. The Tammann diagram created for this effect (Fig. 5c) gives value x = 0.325, which is in an excellent agreement with the theoretical value 0.333 for K2NdBr5. Accordingly, the discussed effect can be ascribed to incongruent melting of K2NdBr5.

In the composition range 0.333 < x < 0.666, only one endothermic peak at 754 K was observed, in addition to the liquidus, on the DSC curves (Fig. 4d). It disappears at x = 0.666, thus suggesting an existence of another compound, namely KNd2Br7, and can be ascribed to the K2NdBr5–KNd2Br7 eutectic. The K2NdBr5–KNd2Br7 eutectic contribution to the enthalpy of fusion, determined and plotted versus the composition in Fig. 5d, gives the eutectic composition x = 0.532. The mixture with the eutectic composition melts with the enthalpy ΔfusHm of about 18.3 kJ mol−1. In the composition range 0.666 < x < 1.0, only one endothermic peak at 802 K was also observed in addition to the liquidus (Fig. 4e). It corresponds to the KNd2Br7–NdBr3 eutectic. The eutectics composition x = 0.689 was determined from the intercept of the two linear parts in Fig. 5e. The corresponding enthalpy of fusion of the eutectic composition was found to be 21.7 kJ mol−1. Analysis of the Tammann plots (Fig. 5) evidences that no solid solutions are formed in the system.

The complete NdBr3–KBr phase diagram is presented in Fig. 6, and all the experimentally determined temperatures of thermal effects are presented in Table 2.
Fig. 6

Phase diagram of the NdBr3–KBr system

Table 2

Results of the DSC experiments performed for the NdBr3–KBr binary system: T1—formation temperature of K3NdBr6, T2—KBr–K3NdBr6 eutectic temperature, T3—temperature of incongruent melting of K2NdBr5, T4—K2NdBr5–KNd2Br7 eutectic temperature, T5—KNd2Br7–NdBr3 eutectic temperature

X(NdBr3)

T1/K

T2/K

T3/K

T4/K

T5/K

Tliquidus/K

0.000

1006

0.051

682

847

980

0.099

680

855

947

0.149

682

852

883

0.199

680

851

0.220

679

846

899

0.240

679

844

914

0.250

683

918

0.270

678

819

913

0.298

680

824

895

0.329

680

824

863

0.350

822

0.396

756

822

0.449

761

798

0.497

759

772

0.550

760

772

0.595

755

800

0.643

751

812

0.650

750

814

0.667

738

814

0.680

805

820

0.692

804

0.721

807

836

0.747

807

851

0.807

802

880

0.850

799

901

0.924

787

933

1.000

954

Our finding can be compared with the Gedlu et al.’s [23] as well as Blachnik and Jaeger-Kasper’s [18] results. It is evident that Gedlu et al.’s [23] results are completely wrong. Although they found two compounds of the same stoichiometry (K3NdBr6 and KNd2Br7), their properties are totally different. According to the authors [23], K3NdBr6 melts incongruently and KNd2Br7 decomposes in the solid state, whereas results of Blachnik and Jaeger-Kasper [18] as well as our findings indicate that these compounds melt congruently. In addition, Gedlu et al. [23] did not find another compound (K2NdBr5) in the system, whereas it was evidenced by Blachnik and Jaeger-Kasper [18] and by us. Our findings are comparable with Blachnik and Jaeger-Kasper’s [18] results. Unfortunately, the latter are presented in a graphical form only. From this graphical presentation, the temperatures of characteristic points as well as eutectic compositions were estimated. The same defined compounds, namely K3NdBr6, K2NdBr5 and KNd2Br7, were found in the system. However, we found that K3NdBr6 was formed from KBr and K2NdBr5 at high temperature (683 K), whereas the literature [18] informs that it is not formation but a solid–solid transition. A significant difference was found in the melting temperature of K3NdBr6, K2NdBr5 and KNd2Br7 compounds. We determined these temperatures as 918 K, 822 and 814 K, respectively, whereas the literature data [18] (929, 828 and 835 K, respectively) are significantly higher. Significant differences were also found in the case of KBr–K3NdBr6, K2NdBr5–KNd2Br7 and KNd2Br7–NdBr3 eutectics. Our finding for the eutectic temperatures (849, 754 and 802 K, respectively) is lower than those presented in the literature [18] (861, 758 and 809 K, respectively). Moreover, our finding for the eutectics compositions (x (NdBr3) = 0.192, 0.532 and 0.689, respectively) differs from those found in the literature data [18] (x (NdBr3) = 0.177, 0.558 and 0.699, respectively).

Conclusions

  1. 1.

    Phase equilibria in the NdBr3–MBr binary systems (M = Na, K) were established by differential scanning calorimetry (DSC). The system with NaBr is a simple eutectic system with two compounds that decompose in the solid state (NaNdBr4 at 603 K and Na3NdBr6 at 580 K). In the system with KBr, three stoichiometric compounds exist. First (K3NdBr6) is formed from KBr and K2NdBr5 at 680 K and melts congruently at 918 K. Second (KNd2Br7) melts congruently at 814 K. Third compound (K2NdBr5) melts incongruently at 822 K.

     
  2. 2.

    The composition of the eutectics was determined with the help of constructed Tammann diagrams. NaBr–NdBr3, KBr–K3NdBr6, K2NdBr5–KNd2Br7 and KNd2Br7–NdBr3 eutectics were found to be located at x = 0.443 (644 K), 0.192 (849 K), 0.532 (754 K) and 0.689 (802 K), respectively.

     
  3. 3.

    Literature data on the systems under investigation were verified, and some of them were found to be completely wrong.

     

Notes

Acknowledgements

The work was financed by a statutory activity subsidy from the Polish Ministry of Science and Higher Education for the Faculty of Chemistry of Wroclaw University of Science and Technology. Financial support by the Algerian Ministry of Higher Education and Scientific Research is gratefully acknowledged. M. B and Y. B wish to thank the Department of Chemistry of Wroclaw University of Science and Technology for the hospitality and support during this work.

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Authors and Affiliations

  1. 1.Laboratoire de Physico-chimie des Matériaux et Catalyse, Faculté des Sciences ExactesUniversité de BejaiaBéjaïaAlgeria
  2. 2.Chemical Metallurgy Group, Department of ChemistryWroclaw University of Science and TechnologyWroclawPoland

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