Abstract
The magnetic properties and magnetocaloric effect (MCE) of ternary intermetallic RE2Cu2Cd (RE = Dy and Tm) compounds and its composite materials have been investigated in detail. Both compounds undergo a paramagnetic to ferromagnetic transition at its own Curie temperatures of TC ~ 48.5 and 15 K for Dy2Cu2Cd and Tm2Cu2Cd, respectively, giving rise to the large reversible MCE. An additionally magnetic transition can be observed around 16 K for Dy2Cu2Cd compound. The maximum values of magnetic entropy change (−ΔSMmax) are estimated to be 17.0 and 20.8 J/kg K for Dy2Cu2Cd and Tm2Cu2Cd, for a magnetic field change of 0–70 kOe, respectively. A table-like MCE in a wide temperature range of 10–70 K and enhanced refrigerant capacity (RC) are achieved in the Dy2Cu2Cd - Tm2Cu2Cd composite materials. For a magnetic field change of 0–50 kOe, the maximum improvements of RC reach 32% and 153%, in comparison with that of individual compound Dy2Cu2Cd and Tm2Cu2Cd. The excellent MCE properties suggest the RE2Cu2Cd (RE = Dy and Tm) and its composite materials could be expected to have effective applications for low temperature magnetic refrigeration.
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Introduction
Magnetic refrigeration technology based on the magnetocaloric effect (MCE) shows superior application potential over conventional gas compression/expansion refrigeration technology because of its environmental friendliness, higher energy efficiency as well as compactness1,2,3,4,5. The MCE is an intrinsic thermal response for the application or removal of a magnetic field to a magnetic material, which can be characterized by the coupled variations of two quantities: the adiabatic temperature change (ΔTad) or/and isothermal magnetic entropy change (ΔSM). To satisfy practical application, extensive efforts have been carried out to pick out the magnetic materials with large/giant MCE as magnetic refrigerants1,2,3,4,5,6,7,8,9,10.
Recently, the rare-earth (RE) based alloys and oxides, which exhibit the large reversible MCEs and refrigeration capacity with small or zero hysteresis have been of great of interest11,12,13,14,15,16,17. Increasing efforts have been devoted for study of the ternary intermetallic compounds of the RE2T2X2:2:1 (T = transition metals and X = III group p-metals). Among of the 2:2:1 system, the RE2Cu2X (X = Mg, Cd, Sn or In) crystallized with the tetragonal Mo2B2Fe-type structure18, have attracted some attentions because of their unique physical and magnetic properties. The basic crystal chemical data of the different RE2T2X series have been reviewed19,20. Very recently, Zhang et al. and Li et al. have reported the large reversible MCEs in RE2Cu2In (RE = Dy, Er and Tm) and Ho2T2In (T = Cu and Au) compounds, respectively21,22,23. However, the systems with the p-metals as cadmium are much less known, what besides other reasons could be explained also by the difficulty in materials synthesis due to the high vapour pressure (low boiling point) of cadmium.
To further understand the physical properties of RE2T2X system, in this paper, the magnetic properties and MCE in RE2Cu2Cd (RE = Dy and Tm) compounds and its composite materials have been investigated systematically. Not only a large reversible MCE was observed in Dy2Cu2Cd and Tm2Cu2Cd compounds, but also an enhanced refrigerant capacity was found in its composite materials.
Results and Discussion
Figure 1(a,b) show the temperature dependence of the zero field cooled (ZFC) and field cooled (FC) magnetization M under different magnetic fields for Dy2Cu2Cd and a magnetic field of 2 kOe for Tm2Cu2Cd, respectively. Both compounds display a typical paramagnetic to ferromagnetic (PM-FM) transition and the Curie temperatures TC, corresponding to the peak of dMFC/dT - T curve [inset of Fig. 1(b)], are determined to be 48.5 K and 15 K for Dy2Cu2Cd and Tm2Cu2Cd, respectively. Another magnetic transition can be observed for Dy2Cu2Cd around TS ~ 16 K under low magnetic fields and it shifts to much lower temperatures with increasing magnetic field. Such behaviours may arise from a spin glass transition or spin reorientation phenomenon24,25, a systematically detail study of the lower temperature magnetic transition will be performed later. The transition temperatures are in good agreement with previously reported values in the literatures20. Figure 2(a,b) show the temperature dependence of the magnetization M (left side) and the reciprocal susceptibility 1/χ (right side) for Dy2Cu2Cd and Tm2Cu2Cd compounds under a magnetic field of 10 kOe, respectively. The 1/χ in paramagnetic regime from 80 to 298 K obeys the Curie-Weiss law for both compounds. The fitted lines are a guide to the eyes for Dy2Cu2Cd and Tm2Cu2Cd compounds as shown in the insets of Fig. 2(a,b), respectively. The fit to the Curie-Weiss formula yields positive paramagnetic Curie temperatures (θP), θP = 45.3 K for Dy2Cu2Cd and θP = 14.1 K for Tm2Cu2Cd, respectively, suggesting dominant ferromagnetic interactions. The effective magnetic moments (μeff) are 10.84 μB and 7.72 μB for Dy2Cu2Cd and Tm2Cu2Cd, respectively. Such moments are close to those of the free ion values of Dy and Tm taking the theoretical RE3+ moment of 10.86 μB and 7.56 μB, respectively.
The magnetic isothermal M(H) curves of Dy2Cu2Cd and Tm2Cu2Cd compounds with increasing field around their transition temperatures with increasing magnetic field up to 70 kOe have been measured and some of them are shown in Figs 3(a) and 4(a), respectively. The magnetization below TC increases rapidly in the low magnetic field range for both compounds and it tends to saturate for Dy2Cu2Cd compound with increasing magnetic field, whereas it is not saturated at 70 kOe for Tm2CuCd compound. To further understand the magnetic transitions, Arrott plots (H/M vs. M2) of Dy2Cu2Cd and Tm2Cu2Cd compounds are shown in Figs 3(b) and 4(b), respectively. According to Banerjee criterion26, the signal (positive and negative) of the slope in Arrott plots has been used to determine the nature of the magnetic phase transition. The negative slopes or inflection points in the Arrott plots often are corresponding to a first order phase transition, whereas the positive slopes are associated to a second order phase transition. By this criterion, neither the inflection points nor negative slopes can be observed in the Arrott plots for Dy2Cu2Cd and Tm2Cu2Cd compounds, indicating a characteristic of the second order (FM-PM) magnetic phase transition.
Figure 5(a,b) show the temperature dependence of magnetic entropy change −ΔSM for Dy2Cu2Cd and Tm2Cu2Cd compounds which is derived from the temperature and field dependence of the magnetization M (H, T) by using the Maxwell’s thermodynamic relation27, , respectively. It can be found that the maximum value of −ΔSM increases monotonically with increasing magnetic field change for both compounds [see insets of Fig. 5(a,b)]. Two successive −ΔSM peaks (one at around TC, another at around TS) can be clearly seen even the low magnetic field change for Dy2Cu2Cd compound, thus obviously enlarging the temperature range of MCE. Only a pronounced peak in the −ΔSM(T) curves is observed around TC for Tm2Cu2Cd compound. For the magnetic field changes of 0–20, 0–50 and 0–70 kOe, the maximum values of the magnetic entropy change (−ΔSMmax) are evaluated to be 7.2, 13.8 and 17.0 J/kg K around TC and 3.3, 6.6 and 8.3 J/kg K around TS for Dy2Cu2Cd compound; and to be 9.2, 17.3 and 20.8 J/kg K for Tm2Cu2Cd compound, respectively.
In addition, the ΔSM (T) curves for the materials with the second order phase transition can be also described using a universal curve28,29, which is constructed by normalizing with their respective maximum value ΔSMmax (i. e. ΔS′ = ΔSM (T)/ΔSMmax) and rescaling the temperature θ, defined as
where the Tr1 and Tr2 are the temperatures of the two reference points of each curve that correspond to 0.6ΔSMmax. The transformed ΔS′ (θ) curves for Tm2Cu2Cd and Dy2Cu2Cd compounds are displayed in Figs 6 and 7, respectively. We can note that all the rescaled ΔSM curves for Tm2Cu2Cd are overlapped with each other in the present temperature range, as shown in Fig. 6, proving the occurrence of the second order magnetic phase transition in Tm2Cu2Cd compound. In parallel, the curves for Dy2Cu2Cd compound are also overlapped with each other around and above TC (see Fig. 7). Whereas an obvious deviation below TC for θ < −2 (around TS) can be found which is properly due to the spin reorientation phenomenon or spin glass transition. Therefore, the ΔSM (T) around TS (5–30 K) are rescaled and the results are shown in the inset of Fig. 7. Similarly, the curves around TS are well overlapped with each other. Furthermore, the rescaled ΔS′ (θ) curves around TC and TS for Dy2Cu2Cd compound under various magnetic field changes are summarized together (as given in the Fig. 8). One can find that all the rescaled ΔSM curves can collapse onto one universal curve, which is consistent with the previous investigations that the materials with successive magnetic phase transitions22,24,30,31. The analysis of the universal behaviour further confirms that the Dy2Cu2Cd compound with the second order phase transition.
Another important quality factor of refrigerant materials is the refrigerant capacity [RC, defined as numerically integrating the area under the −ΔSM - T curve at full width of half maximum (δFWHM) of the −ΔSM peak as the integrating limits]. For the magnetic field changes of 0–20, 0–50 and 0–70 kOe, the values of RC are evaluated to be 87, 316 and 495 J/kg for Dy2Cu2Cd compound; and to be 60, 165 and 248 J/kg for Tm2Cu2Cd compound, respectively. It is well known that magnetic refrigeration systems based on an ideal Ericsson cycle requires a magnetocaloric material with a constant ΔSM over an operating refrigeration temperature range32,33. Besides the materials with successive magnetic transitions or with a very magnetic field sensitive magnetic phase transitions22,24,30,31,34, composite materials have been considered to be the most promising method to accomplish the requirement of Ericsson cycle since it can lead to almost constant ΔSM with enlarged temperature span35,36,37,38. An enhanced RC have been successfully realized in Eu8Ga16Ge30-EuO36, amorphous FeZrB(Cu)37 and ErNiBC-GdNiBC38 composite materials. We can note that the Dy2Cu2Cd and Tm2Cu2Cd compounds possess the same crystal structure with similar lattice parameters and similar magnitudes of the magnetic entropy change (−ΔSM). Therefore, these composite materials could be expected to fulfil the required Ericsson cycle conditions. The total magnetic entropy change of x Dy2Cu2Cd + (1 − x) Tm2Cu2Cd composite materials, ΔScomp(T, H, x), can be calculated theoretically from the individual ΔSM(T) curves35,36,37,38,
where x and 1 − x are the weight amounts of Dy2Cu2Cd and Tm2Cu2Cd, respectively. Based on both compounds, a composite material can be formed and the optimum ratio of x ~ 0.77 is determined by using a numerical method. The magnetic entropy change ΔScomp(T) for Dy2Cu2Cd - Tm2Cu2Cd composite material at x ~ 0.77 under a magnetic field change of 0–50 kOe is shown in Fig. 9. A table-like MCE in a wide temperature span of 10–70 K can be observed in ΔScomp(T) curve which is desirable for an ideal Ericsson-cycle magnetic refrigeration. The corresponding maximum value of RCcomp is 417 J/kg, which is 32% and 153% higher than those of Dy2Cu2Cd (316 J/kg) or Tm2Cu2Cd (165 J/kg). The transition temperature TC, the maximum values of −ΔSMmax and RC under the magnetic field change of 0–50 kOe for Dy2Cu2Cd and Tm2Cu2Cd as well as the 0.77 Dy2Cu2Cd - 0.23 Tm2Cu2Cd composite material together with some MCE materials in the similar working temperature range are listed in Table 1 for comparison. The MCE parameters for the present studied materials are comparable or larger than those of other potential magnetic refrigerant materials in the similar temperature region, suggesting RE2Cu2Cd composite materials could be a promising candidate for magnetic refrigeration for Ericsson cycle in the temperature range of 10–70 K. The present results allow for the possibility of using RE2Cu2Cd compounds to fabricate composite materials with desirable magnetocaloric properties for active magnetic refrigeration.
Conclusions
In summary, two single phased Dy2Cu2Cd and Tm2Cu2Cd compounds have been fabricated and the magnetism and magnetocaloric effect have been investigated experimentally. Both compounds undergo a paramagnetic to ferromagnetic transition at their own Curie temperatures, additionally, another magnetic transition is also observed for Dy2Cu2Cd at low temperatures. For a magnetic field change of 0–50 kOe, the maximum values of magnetic entropy change (−ΔSMmax) are 13.8 J/kg K around TC and 6.6 J/kg K around TS for Dy2Cu2Cd; and 17.3 J/kg K for Tm2Cu2Cd, respectively. The rescaled entropy change ΔSM curves around TC follow a universal behaviour for Dy2Cu2Cd and Tm2Cu2Cd, which further confirm both compounds with the second order phase transition. A table-like MCE from 10 to 70 K and a strong enhancement of RC have been found in theoretically calculated Dy2Cu2Cd-Tm2Cu2Cd composite materials. The maximum value of RCcomp is 417 J/kg in the 0.77Er2Cu2Cd - 0.23Tm2Cu2Cd composite material for a magnetic field change of 0–50 kOe, which is obviously larger than those for either Dy2Cu2Cd (316 J/kg) or Tm2Cu2Cd (165 J/kg) compounds. The results indicate that the RE2Cu2Cd (RE = Dy and Tm) compounds and its composite materials could be promising candidates for magnetic refrigeration in the temperature range of 10–70 K. Furthermore, the present results may also provide a cost-effective strategy for exploring suitable refrigeration candidates with table-like magnetocaloric feature by a materials composition method, beneficial for Ericsson-cycle in the wide temperature range.
Methods
The Dy2Cu2Cd and Tm2Cu2Cd polycrystallize samples were fabricated by induction melting the elements in a sealed quartz crucible. Firstly, high purity Dy, Tm, Cu and Cd with stoichiometric amounts were weighted and placed in the quartz crucible. Secondly, a high vacuum better than 2*10−5 mbar was achieved in the crucible. Then the crucible was filled with purified argon gas at pressure of ca. 750 mbar and sealed immediately. Finally, the quartz crucible was placed in an induction furnace and heated at 1100 K for 4 minutes, following by 3 hours annealing at 850 K. The powder X-ray diffraction (Bruker D8 Advance) measurements were carried out at room temperature using Cu Kα radiation. Both samples were proved to be single phase and the lattice parameters were evaluated to be a = 7.491 and c = 3.742 Å for Dy2Cu2Cd; and to be a = 7.439 and c = 3.687 Å for Tm2Cu2Cd, respectively. The magnetic measurements were performed by using a commercial vibrating sample magnetometer (VSM) which is an option of the physical properties measurement system (PPMS-9, Quantum Design) in the temperature range of 3–298 K with a DC magnetic field from 0 to 7 T and the samples are small particles of 4.5 and 3.8 mg for Dy2Cu2Cd and Tm2Cu2Cd, respectively.
Additional Information
How to cite this article: Zhang, Y. et al. Excellent magnetocaloric properties in RE2Cu2Cd (RE = Dy and Tm) compounds and its composite materials. Sci. Rep. 6, 34192; doi: 10.1038/srep34192 (2016).
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Acknowledgements
The present work was partially supported by the National Natural Science Foundation of China (No. 51501036). Y. K. Zhang acknowledges the Alexander von Humboldt (AvH) Foundation for support with a post-doctoral fellowship.
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Y.Z. designed the study. Y.Y., X.X., S.G. and L.H. prepared the samples and preformed the magnetocaloric measurements. Z.R., X.L. and G.W. provided suggestions for the data analyses and the manuscript. Y.Z. prepared the manuscript and all authors reviewed the manuscript.
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Zhang, Y., Yang, Y., Xu, X. et al. Excellent magnetocaloric properties in RE2Cu2Cd (RE = Dy and Tm) compounds and its composite materials. Sci Rep 6, 34192 (2016). https://doi.org/10.1038/srep34192
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DOI: https://doi.org/10.1038/srep34192
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