Article pubs.acs.org/jced
Electrical Conductivity of LiCl−KCl−CsCl Melts Jinze Li, Bingliang Gao,* Wenting Chen, Chengyuan Liu, Zhongning Shi, Xianwei Hu, and Zhaowen Wang School of Metallurgy, Northeastern University, Shenyang 110819, China S Supporting Information *
ABSTRACT: The electrical conductivities of ternary mixtures of LiCl−KCl−CsCl (xLiCl = 0.575 in mole fraction) were investigated by the impedance method in a capillary cell below 723 K. It showed that the electrical conductivities of the ternary melt decreased significantly with increasing molar fraction of CsCl.
used for thermal batteries. Ishii et al.25 investigated the thermal conductivity of LiF, NaF, KF and their mixtures. The density and electrochemical window of LiCl−KCl−CsCl melts were measured by Ito.26,27 However, the electrical conductivities of LiCl−KCl−CsCl melts have not been found in the literature. In this study, the electrical conductivities for different compositions of the LiCl−KCl−CsCl system have been measured by the impedance method in a capillary cell below 723 K.
1. INTRODUCTION Alkali metal chloride salts and their mixtures have been widely used as solvents for electrochemical applications1−5 because of their superior properties, such as high electrical conductivity, good thermal and chemical stabilities, relatively low liquidus temperature, and a wide electrochemical window. The electrochemical studies and electrodeposition have been performed in two alkali-metal halides: LiCl−KCl (58.5:41.5 in mole fraction, m. p., 625 K) and LiF−KF−NaF (46.5:11.5:42.0 in mole fraction, m. p., 732 K).6−9 Besides these two mixtures, other alkali metal halide mixtures, such as NaCl−KCl (50:50 in mole fraction) and LiCl−KCl−NaCl (55:36:9 in mole fraction), have also been applied as electrolyte in electrochemical applications.10,11 In some electrochemical applications, a lower operation temperature is more favorable for an electrolyte because of a wider range of material selection and possibilities of new energy conversion systems. Ito and Nohira suggested some new molten salts with low melting points: LiBr−KBr−CsBr eutectic (56.1:18.9:25.0 in mole fraction, m. p., 498 K), LiCl−KCl− CsCl eutectic (57.5:13.3:29.2 in mole fraction, m. p., 538 K) and ZnCl2−NaCl−KCl eutectic (60:20:20 in mole fraction, m. p., 476 K).5,12 In recent years, LiCl−KCl−CsCl melts have been applied as electrolyte for electrodeposition of refractory metals,13−15 formation of metal nanoparticles,16−18 and electrochemical synthesis.19−21 The physical and chemical properties of alkali metal chloride salt mixtures have been reviewed by Janz.22,23 Among these systems, the binary eutectic LiCl−KCl melt is one of the mostly studied systems. Additionally, some ternary and quaternary alkali halide salts have already been studies by researchers. Masset and Guidotti24 reviewed the physical and chemical properties of the ternary and quaternary systems of molten salts © XXXX American Chemical Society
2. EXPERIMENTAL SECTION 2.1. Chemicals. Chemicals, used in this work, and their information are listed in Table 1. All chemicals were dried in a vacuum oven at 473 K for 6 h before the measurement of the electrical conductivity. In the case of lithium chloride, it was heated at 333 K for 24 h and at 473 K for 6 h under vacuum condition. The mixtures were weighed and mixed in a glove box (MBRAUN MB 200B, Germany) filled with high purity of argon. The standard uncertainty in the compositions is 0.001 in mole fraction. 2.2. Apparatus and Measurements. The electrical conductivities of the melts were measured by the impedance method in a capillary cell. The schematic graph of the experimental apparatus is shown in Figure 1. The capillary cell used for the measurement was made of a corundum tube (8 mm outer diameter, 500 mm length, Shenyang Tianhong Ceramic Material Co., Ltd., Al2O3 > 0.99 in mass fraction), which has two longitudinal channels for the platinum working electrodes made of 0.9999 (in mass fraction) pure platinum Received: August 10, 2015 Accepted: February 24, 2016
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DOI: 10.1021/acs.jced.5b00682 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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Table 1. Chemical Information chemical name
source
initial mass fraction purity
lithium chloride potassium chloride cesium chloride potassium nitrate sodium nitrate
Alfa Aesar Alfa Aesar Sigma-Aldrich Sinopharm Chemical Reagent Co., Ltd. Sinopharm Chemical Reagent Co., Ltd.
0.999 0.99997 0.99 0.99 0.99
purification method vacuum vacuum vacuum vacuum vacuum
final mass fraction purity
drying drying drying drying drying
analysis method none none none none none
digital thermometer with a resolution of 0.1 K. All experiments were done by placing the lower part of the quartz crucible in the constant temperature zone of the furnace. The K type thermocouple was calibrated to the melting points of pure KNO3 and LiCl. The measured transition temperatures were reproducible to within ±1 K. Argon gas was passed through the quartz crucible at a rate of 1 L·min−1. It is well-known that lithium chloride has an ability to absorb water and undergo hydrolysis when being heated, which may have a negative impact on the reliability of the experimental values. The electrical conductivity of lithium chloride was measured using the same method. After a conductivity measurement, the pH of the lithium chloride aqueous solution was checked. The pH of the LiCl solution (1 M) was 7.15 for the upper layer of the solid melt and 6.58 for the lower layer of the solid melt, which was little higher than that of the starting material (the pH of 1 M solution was 6.42). The results indicate that water absorption and hydrolysis were almost restrained during conductivity measurement.
Figure 1. Schematic diagram of the apparatus for electrical conductivity measurement: (a) corundum tube for gas inlet and outlet, (b) thermocouple, (c) molten salt, (d) Pt wires, (e) capillary cell, (f) quartz crucible.
3. RESULTS AND DISCUSSION The liquidus temperatures for mixtures of LiCl−KCl−CsCl, determined from the first thermal delay in their TA traces, are presented in Table 2. The melting point for the ternary eutectic composition (LiCl/KCl/CsCl = 57.5:13.3:29.2 in mole fraction) is 537.6 K, which agrees with the reported data of 538 K.26
wire measuring 0.3 cm in diameter. The Pt wires were fixed at the top of the corundum tube using modified acrylate adhesive. The lower tips of the electrodes were in a plane parallel with the melt surface. A K type thermocouple with silica shielding was dipped in the melt for measuring the temperature of the molten salts. A quartz crucible was used as electrolyte container that was hermetically closed by a stopper. The interior dip cell was fixed to the stopper. The quartz crucible was transferred into a furnace and heated up to the measurement temperature. The resistance of the melting salt was measured with a LCR meter (Agilent 4263B) at a fixed frequency of 1000 Hz and a voltage of 1 V. The electrical conductivity (κ) was calculated according to the following equation:
Table 2. Liquidus Temperatures of Selected Compositions in the System of LiCl−KCl−CsCl at 101.325 kPaa
C (1) R −1 where C is the cell constant in cm , which was determined by using aqueous potassium chloride solution (1 mol·L−1) at room temperature. R is the measured resistance in Ω. The cell constant C of the capillary cell was 136.6 cm−1 and calibrated using potassium nitrate melt within a temperature range of 613 to 673 K. Compared to the reference values given by G. D. Robbins and J. Braunstein,28 the deviation is less than 1%. The temperature range for the conductivity measurement is from the liquidus temperature of the investigated melt to 723 K. The liquidus temperatures of the investigated melts were determined by the thermal analysis (TA), which was performed under an atmospheric pressure of argon in the same quartz crucible with ports for thermocouple and argon gas inlet. The cooling rate was 1 K·min−1. The temperature of the melt was measured by immersing a type K thermocouple connected to a κ=
composition (in mole fraction) LiCl/KCl/CsCl
liquidus temp (K)
57.5:0:42.5 57.5:8.2:34.3 57.5:13.3:29.2 57.5:16.4:26.1 57.5:24.6:17.9 57.5:32.8:9.7 57.5:41.0:1.5
593.0 567.0 537.6 544.0 561.5 596.3 623.7
a
Standard uncertainties u for temperature T, pressure P, and mole fraction x are u(T) = 0.1 K, u(P) = 1 kPa, u(x) = 0.001. Relative standard uncertainty ur for the liquidus temperature Liq. T is ur(Liq. T) = 0.01.
For evaluating accuracy of the data obtained in this work, the electrical conductivities of pure KNO3 and NaNO3 were measured by the method mentioned above and the results were compared with the data from refs 28 and 29, which are shown in Figure 2. All the data is also presented in Tables S1 and S2. In our study, the investigated temperature range for the LiCl− KCl−CsCl systems was between 563 and 723 K, which is close to that of KNO3 melt and NaNO3 melt. The deviations for both nitrates measured in this study were less than 1%. It is well-known that the cell constant is a temperature-dependent B
DOI: 10.1021/acs.jced.5b00682 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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Figure 2. Comparison between the electrical conductivities of pure NaNO3 and KNO3 in this work and data from different references: (red ○) KNO3 (in this work); (■) KNO3 (ref 28); (blue □) KNO3 (ref 29, page 594); (green ▲) NaNO3 (in this work); (purple △) NaNO3 (ref 29, page 619).
Figure 4. Comparison between the electrical conductivities of LiCl− CsCl (57.5:42.5 in mole fraction) and LiCl−CsCl (58:42 in mole fraction): (black ■) ref 22 for LiCl−CsCl (58:42 in mole fraction); (blue △) LiCl−CsCl (58:42 in mole fraction), in which CsCl was used without recrystallization treatment; (red ●) LiCl−CsCl (58:42 in mole fraction), in which CsCl was used with recrystallized CsCl; (pink ▲) LiCl−CsCl (57.5:42.5 in mole fraction).
value. These results indicate that the impact of temperature on cell constant can be neglected in the investigated temperature range. On the basis of the above analysis, the relative standard uncertainty for electrical conductivity in the investigated temperature range is 0.01 with 0.68 level of confidence. The electrical conductivities vs temperature for the mixtures of ternary alkali metal chlorides were measured in this work and presented in Table S3. The temperature dependence of electrical conductivity for all mixtures, as shown in Figure 3,
shown in Figure 4. Because of the relatively lower purity of CsCl, the influence of impurities in CsCl on conductivity measurement was checked. The electrical conductivity of LiCl− CsCl (58:42 in mole fraction) was remeasured with recrystallized CsCl. The difference is small enough to neglect the influence of impurity in CsCl. The significant difference between our data and ref 22 may be due to the different apparatus of measurements. It deserves a reinvestigation of the electrical conductivity of the LiCl−CsCl system, which will be given in our future work. All the data shown in Figure 4 is presented in Table S4. In the temperature range of 563 to 723 K, the experimental data were least-squares fitted to equations of the form κ = a + bT + cT 2 (ohm−1 cm−1)
(2)
where T is temperature in K. The obtained parameters a, b and c are given in Table 3. As the squared values are larger than 0.999, the above equations fit the experimental data very well. Table 3. Parameters of Equation 2 for LiCl−KCl−CsCl Systems composition (mole fraction)
Figure 3. Temperature dependence of electrical conductivity for the LiCl−KCl−CsCl molten salts in mole fraction: (black □) 57.5:0:42.5; (red ●) 57.5:8.2:34.3; (blue ★)57.5:13.3:29.2 (eutectic); (red ○) 57.5:16.4:26.1; (green ▽) 57.5:24.6:17.9; (blue △) 57.5:32.8:9.7; (purple ◇) 57.5:41.0:1.5.
is nearly linear increasing with the increase of temperature. The electrical conductivities of the ternary mixtures increase with increasing KCl and decreasing CsCl at fixed concentration of LiCl (xLiCl = 0.575 in mole fraction). In Figure 4, there is a significant difference between the electrical conductivity of LiCl−KCl−CsCl (57.5:0:42.5 in mole fraction) obtained in this work and that of LiCl−CsCl (58:42 in mole fraction) from ref 22. In general, a very small composition difference should not make such a large deviation. The electrical conductivity of LiCl−CsCl (58:42 in mole fraction) was measured in this work and presented in Figure 4 too. The result is also much smaller than the data from ref 22 as
temp range
κ = a + bT + cT2 (K) (S·cm−1)
LiCl/KCl/CsCl
a
b·103
c·106
adj. R2
K
57.5:0.0:42.5 57.5:8.2:34.3 57.5:13.3:29.2 57.5:16.4:26.1 57.5:24.6:17.9 57.5:32.8:9.7 57.5:41.0:1.5
−2.144 −1.768 −1.538 −1.436 −2.506 −4.084 −7.449
3.640 2.330 1.640 1.340 4.550 9.220 19.700
0.761 1.999 2.583 2.827 0.698 −2.277 −9.902
0.9999 0.9997 0.9996 0.9997 0.9998 0.9996 0.9991
603−723 578−723 563−723 563−723 563−723 598−723 623−723
These conductivities were fitted by the Arrhenius equation: ⎡ −E ⎤ κ = A exp⎢ a ⎥ ⎣ RT ⎦
(3)
where A is pre-exponential factor, Ea is activation energy, and T is temperature in K. C
DOI: 10.1021/acs.jced.5b00682 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
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In addition, the phase equilibrium study of the LiCl−CsCl system indicated the existence of two congruently melting compounds: LiCl·CsCl and LiCl·2CsCl.31 Some Li−Cl−Cs complexes may exist in the melt when the temperature is below 623 K. The significant decreasing of conductivity may be a result of the presence of the complexes. The complex breaks down as the temperature increases and the proportion of ions, that is, Li+ and Cs+, becomes higher, increasing the conductivity. The classic ionic melt originates at temperatures far above the liquidus temperature point.
The data for the tested melts are shown in Figure 5. It shows that the Arrhenius equation over the temperature range 623 to
4. CONCLUSIONS The electrical conductivities for the ternary alkali metal chloride molten salts LiCl−KCl−CsCl were studied at temperatures ranging from 563 to 723 K. The electrical conductivity of the ternary melts decreased with increasing molar fraction of CsCl when the content of LiCl is fixed at 57.5 in mole fraction. Some Li−Cl−Cs complexes may exist in the melt when temperature is below 623 K.
■
Figure 5. Arrhenius plots for the tested LiCl−KCl−CsCl melts in mole fraction: (black □) 57.5:0:42.5; (red ●) 57.5:8.2:34.3; (blue ★) 57.5:13.3:29.2; (red ○) 57.5:16.4:26.1; (green ▽) 57.5:24.6:17.9; (blue △) 57.5:32.8:9.7; (purple ◇) 57.5:41.0:1.5.
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jced.5b00682. Electrical conductivity data of LiCl−KCl−CsCl melts obtained in this work, electrical conductivity data of pure NaNO3 and KNO3, and electrical conductivity data of LiCl−KCl melts (PDF)
723 K is well obeyed. Out of the range, the data have a negative deviation from the Arrhenius plots. The activation energies (Ea) and the parameter A are listed in Table 4. They indicate that Table 4. Ea and A Calculated from the Arrhenius Equation composition (mole fraction) LiCl/KCl/CsCl
Ea (J·mol−1)
A
temp range (K)
57.5:0.0:42.5 57.5:8.2:34.3 57.5:13.3:29.2 57.5:16.4:26.1 57.5:24.6:17.9 57.5:32.8:9.7 57.5:41.0:1.5
26.397 25.050 24.285 24.327 23.554 21.808 18.524
72.603 62.240 56.770 57.974 58.323 53.250 35.909
643−723 658−723 658−723 658−723 633−723 623−723 623−723
ASSOCIATED CONTENT
S Supporting Information *
■
AUTHOR INFORMATION
Corresponding Author
*E-mail:
[email protected]. Funding
The authors would like to express their gratitude for the financial support provided by the NEU Foundation (Grant No. N130402011), the National Natural Science Foundation of China (Grant No. 51574070, 51474060). Notes
The authors declare no competing financial interest.
■
the activation energies (Ea) present an increasing trend with increasing amount of CsCl. Regarding the pure chemicals used in this system, CsCl has the activation energy of 4.293 J·mol−1 in the temperature range of 926 to 1170 K, which is larger than that of KCl (2.295 J·mol−1, 1052 to 1373 K) and LiCl (1.469 J· mol−1, 896 to 1056 K).23 The activation energy of electrical conductance of their mixture has a significantly higher value, which indicates the important role of temperature and ionic structures of melt on electrical conductance. According to the molecular dynamics simulation of the molten ternary system (Li, K, Cs) Cl from Matsumiya,30 when xCs is lower than 0.4, the self-exchange velocity (SEV) of Cs+ is lower than the other two cations in the tested melts. On the other hand, the molar volume of the LiCl−KCl−CsCl melts and the average Cl−−Cl− distance increases with increasing content of CsCl. Combined with impact of temperature, some kind of big complexes might form in the investigated melt. Consequently, this leads to a higher energy barrier for ionic conductance with an increase of CsCl content. In summary, it needs more energy to separate the alkali metal cation from the anion and to activate ions to transport electrons. Thus, the activation energy is higher when the concentration of Cs+ is higher.
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DOI: 10.1021/acs.jced.5b00682 J. Chem. Eng. Data XXXX, XXX, XXX−XXX
