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B2576 - Thermal stability of LiPF6based electrolyte and effect of contact with various delithiated cathodes of Li-ion batteries
Thermal stability of LiPF6based electrolyte (1M LiPF6/EC +DMC) was studied by insitu FTIR spectroscopy and C80 calorimetry, which indicated that the electrolyte underwent furious polymerization and decomposition reactions and sharp heat flow was generated below 225 ?C. The thermal stability of the electrolyte in contact with various delithiated cathodes (LixCoO2, LixNi0.8Co0.15Al0.05O2, LixNi1/3Co1/3Mn1/3O2, LixMn2O4, LixNi0.5Mn0.5O2, LixNi0.5Mn1.5O4 and LixFePO4) was also investigated by C80 calorimetry. The results showthat the cathodematerials except for LixFePO4 usually have an enhancement effect on the decomposition of the electrolyte, but LixFePO4 exhibits a suppression effect on the reactions of the electrolyte. LixFePO4 is found to bewith excellent thermal stability. Among the other cathodes, LixCoO2, LixNi0.8Co0.15Al0.05O2, LixNi0.5Mn0.5O2 and LixNi0.5Mn1.5O4 promote the decomposition of electrolyte by releasing oxygen and thus considered not favorable for safety, but LixNi1/3Co1/3Mn1/3O2 with a lesser reaction heat and LixMn2O4 with even less heat flowin the lowtemperature range (50Ð225 ?C) are believed as promising cathodes for better safety. By comparing Xray diffraction (XRD) patterns of these cathode materials at room temperature and those heated to 300 ?C in the presence of the electrolyte, we have found that LixFePO4 only has experienced tiny structure change, which is greatly different from the other cathode materials.
H.F. Xiang, H.Wang, C.H. Chen, X.W. Ge, S. Guo, J.H. Sun, W.Q. Hu, Journal of Power Sources 191 (2009) 575Ð581
B2575 - Cresyl diphenyl phosphate effect on the thermal stabilities and electrochemical performances of electrodes in lithium ion battery
To improve the safety of lithium ion battery, cresyl diphenyl phosphate (CDP) is used as a flame-retardant additive in a LiPF6 based electrolyte. The electrochemical performances of LiCoO2/CDP-electrolyte/Li and Li/CDP-electrolyte/C half cells are evaluated. The thermal behaviors of Li0.5CoO2 and Li0.5CoO2ÐCDP-electrolyte, and LixC6 and LixC6ÐCDP-electrolyte are examined using a C80 micro-calorimeter. For the LiCoO2/CDP-electrolyte/Li cells, the onset temperature of single Li0.5CoO2 is put off and the heat generation is decreased greatly except the one corresponding to 5% CDP-containing electrolyte. When Li0.5CoO2 coexists with CDP-electrolyte, the thermal stability is enhanced. CDP improves the thermal stability of lithiated graphite anode effectively and the addition of 5% CDP inhibits the decomposition of solid electrolyte interphase (SEI) films significantly. The electrochemical tests on LiCoO2/CDP-electrolyte/Li and Li/CDP-electrolyte/C cells show that when less than 15% CDP is added to the electrolyte, the electrochemical performances are not worsen too much. Therefore, the addition of 5Ð15% CDP to the electrolyte almost does not worsen the electrochemical performance of LiCoO2 cathode and graphite anode, and improves theirs thermal stability significantly; thus, it is a possible choice for electrolyte additive.
Qingsong Wang, Ping Ping, Jinhua Sun, Chunhua Chen, Journal of Power Sources, 196 (2011) 5960Ð5965
B2574 - Improved thermal stability of lithium ion battery by using cresyl diphenyl phosphate as an electrolyte additive
To enhance the safety of lithium ion battery, cresyl diphenyl phosphate (CDP) is explored as an additive in 1.0 M LiPF6/ethylene carbonate (EC) + diethyl carbonate (DEC) (1:1 wt.). The electrochemical performances of LiCoO2/CDP-electrolyte/C cells are tested. At the thermal aspect, the thermal stability of the electrolyte with CDP is detected firstly by using a C80 micro-calorimeter, and then the charged LiCoO2/CDP-electrolyte/C cells are disassembled and wrapped to detect the thermal behaviors. The results indicate that CDP-containing electrolyte enhances the thermal stabilities of electrolyte and lithium ion battery, and the electrochemical performances of LiCoO2/CDP-electrolyte/C cell become slightly worse by using CDP in the electrolyte. Furthermore, the cell with 10% (wt.) CDP-containing electrolyte shows better cycle efficiency than that of other CDP-containing electrolyte, such as containing 5% (wt.) CDP and 15% (wt.) CDP. This maybe because that the mass ratio between CDP and electrolyte is close to the reaction stoichiometric ratio in the 10% (wt.) CDP-containing electrolyte, where stable solid electrolyte interphase (SEI) is formed. Therefore, 10% CDP-containing electrolyte improves the safety of lithium ion battery and keeps its electrochemical performance
Qingsong Wang, Ping Ping, Jinhua Sun, Chunhua Chen, Journal of Power Sources, 195 (2010) 7457Ð7461
B2573 - The effect of mass ratio of electrolyte and electrodes on the thermal stabilities of electrodes used in lithium ion battery
The mass ratio between electrode and electrolyte in lithium-ion battery plays a key role for the battery thermal stability. Its effect on the thermal stability of their coexisting system was studied using C80 micro-calorimeter. For the Li0.5CoO2ÐLiPF6/ethylene carbonate (EC) + diethyl carbonate (DEC) coexisting system, when the mass ratios of Li0.5CoO2ÐLiPF6/EC + DEC are 2:1, 1:1, 1:2 and 1:3, one, two, three and four main exothermic peaks are detected with total heat generation of ?1043.8 J g?1, ?1052.6 J g?1, ?1178.5 J g?1 and ?1684.5 J g?1, respectively. For the LixC6ÐLiPF6/EC + DEC coexisting system, the thermal behavior trend is similar, and the heat generation increases with the electrolyte content increasing, however, and the onset temperature are very close to each others. The heating rate also influence the heat generation rate for the two coexisting system, too far or too low heating rate could results in varies heat generation.
Qingsong Wang, Ping Ping, Jinhua Sun, Chunhua Chen, Thermochimica Acta, 517 (2011) 16Ð23
B2572 - Enhancing the safety of lithium ion batteries by 4-isopropyl phenyl diphenyl phosphate
To enhance the safety of lithium ion batteries, 4-isopropyl phenyl diphenyl phosphate (IPPP) was explored as an additive in 1.0 M LiPF6/ethylene carbonate (EC)+diethyl carbonate (DEC) (1:1 wt.%). The electrochemical performances of LiCoO2/IPPP electrolyte/C cells were tested. And then the LiCoO2/IPPP electrolyte/C cells were disassembled and wrapped to detect the thermal behaviors using a C80 microcalorimeter. The results indicated that 5% and 10% IPPP content in the electrolyte can enhance the safety of lithium ion batteries. Furthermore, the electrochemical performances of LiCoO2/IPPP electrolyte/C cells become slightly worse by using 5% and 10% IPPP content electrolyte. Therefore, 5Ð10% IPPP content in electrolyte can enhance the safety of lithium ion batteries with minimum sacrifice in electrochemical performance.
Qingsong Wang, Jinhua Sun, Materials Letters 61 (2007) 3338Ð3340
B2571 - Enthalpy of Solution of Carbon Dioxide in Aqueous Solutions of Monoethanolamine at Temperatures of 322.5 K and 372.9 K and Pressures up to 5 MPa
The enthalpies of solution (?solH) of carbon dioxide (CO2) in two aqueous solutions (w = 0.1500 and w = 0.3000) of monoethanolamine (MEA) have been measured at two temperatures (322.5 K and 372.9 K) and pressures up to 5 MPa. Measurements were carried out by a flow calorimetric technique using a custom-made flow-mixing unit combined with a SETARAM C-80 isothermal differential heat-flux calorimeter. Enthalpies of solution of CO2 (?solH) have been obtained as function of loading R (moles CO2/mol amine). Solubility data of the gas into the different absorbent (s) were derived from the enthalpic data.
Hugues Arcis, Karine Ballerat-Busserolles, Laurence Rodier, Jean-Yves Coxam, J. Chem. Eng. Data 2011, 56, 3351Ð3362
B2570 - Studies of heterogeneous interactions between N-acetyl-N?-methyl-l-?-amino acid amides and urea molecules in water at 298.15 K
The enthalpies of solution of N-acetyl-N?-methyl-l-?-threoninamide, N-acetyl-N?-methyl-l-?-tyrosinamide, N-acetyl-N?-methyl-l-?-histidinamide, N-acetyl-N?-methyl-l-?-tryptophanamide have been measured in water and in aqueous urea solutions at 298.15 K. The mixing enthalpies of aqueous urea solution with aqueous N-acetyl-N?-methyl-l-?-valinamide solution and their respective enthalpies of dilution by water have been determined at 298.15 K. The experimental results were used to obtain the enthalpic coefficients of the interaction between amino acid amides and urea molecules in water based on McMillanÐMayer's model. The values of the interaction parameters were interpreted in terms of the hydrophobic or hydrophilic properties of the amino acid radicals in the examined amide molecules and the influence on their interactions with a urea molecule in water
Sylwia Belica, Bart?omiej Pa?ecz, Bo?enna Nowicka, Henryk Piekarski, Andrzej J--?wiak, Thermochimica Acta, 501 (2010) 19Ð23
B2569 - A DSC study of deterioration caused by environmental chemical pollutants to parchment, a collagen-based material
A DSC study of new parchments exposed at 25 ¡C for 1Ð16 weeks to controlled atmospheres containing 50 ppm of gaseous chemical pollutants (NO2, SO2, NO2 + SO2) and 50% relative humidity (RH) was performed. Samples were exposed to chemical pollutants alone, as well as after previous heating at 100 ¡C for 2Ð16 days and/or irradiating with visible light (1.7 ? 105 lx) for 4Ð16 h. DSC measurements were performed in both sealed crucibles in static air atmosphere at 25Ð200 ¡C and open crucibles under gas flow (nitrogen, oxygen, synthetic air) at 25Ð280 ¡C. Analysis of DSC curves provided the variation induced by ageing on the thermodynamic parameters associated with both parchment denaturation and softening of collagen crystalline fraction. All the ageing procedures decreased both temperature and enthalpy of denaturation and increased broadness of DSC peak in function of ageing time. The occurrence of thermal oxidation peaks and/or lower temperature endothermic peaks was observed. The temperature of the first softening peak always indicated a general tendency to decrease as a function of ageing time. Shrinkage temperature of collagen fibres measured by thermomicroscopy also decreased as a result of accelerated ageing treatments.
Petru Budrugeac, Elena Badea, Giuseppe Della Gatta, Lucretia Miu, Alina Com?nescu, Thermochimica Acta, 500 (2010) 51Ð62
B2568 - Nanoceria Energetics of Surfaces, Interfaces and Water adsorption
The surface and interface enthalpies of CeO2 were studied by high temperature oxide melt solution calorimetry combined with water adsorption calorimetry.
Shmuel Hayun, Tatiana Y. Shvarevaa, Alexandra Navrotsky, J.Am. Ceram. Soc. 94 (2011) 3992-3999
B2567 - Hydrogen sorption performance of MgH2 doped with mesoporous nickel- and cobalt-based oxides
The effect of mesoporous Co3O4, NiCo2O4 and NiO on the hydrogen sorption performance of MgH2 was investigated. These oxides were synthesized by multi-step nanocasting and introduced during the high-energy ball milling of MgH2 powder to act as catalysts. Hydrogen desorption on the as-milled powders was assessed upon heating the samples from room temperature to 400 ¡C. In all cases, the onset temperature for desorption was lowered by taking advantage of the introduced additives. The NiO-doped sample displayed the best response, the desorption rate being 7 times faster than in pure MgH2. Complementary kinetic studies on this particular sample revealed that the sorption activation energies were much lower (50 kJ/mol for absorption and 335 kJ/mol for desorption) than the corresponding ones for undoped MgH2 (57 kJ/mol for absorption and 345 kJ/mol for desorption), thus proving the catalytic activity of the mesoporous NiO oxide. Significantly, the X-ray powder diffraction (XRPD) patterns taken on the NiO-doped sample after discharging/charging cycles revealed that Mg could fully hydrogenate at the end of the charging process, while Mg metal was still detected in the undoped (pure) sample. Favored conditions for dissociative chemisorption of hydrogen could be ascribed to the formation of metallic Ni arising from complete or partial reduction of NiO, as observed in the XRPD patterns.
Moiss Cabo, Sebastiano Garroni, Eva Pellicer, Chiara Milanese, Alessandro Girella, Amedeo Marini, Emma Rossinyol, Santiago Suri-ach, Maria Dolors Bar--, International Journal of Hydrogen Energy, 36 (2011) 5400Ð5410
B2566 - Critical assessment and optimization of the AgÐAuÐPb system
By means of an optimization procedure, the ternary AgÐAuÐPb system has been assessed. All available experimental data of the ternary system and the results derived from thermodynamic descriptions for the three limiting binary systems are used. For the AgÐAu and AuÐPb systems, optimized Gibbs energy expressions were taken from the literature. A new assessment of the binary AgÐPb system based on our calorimetric investigations is presented in this paper.Calculated phase diagrams and some calculated thermochemical functions for the binary AgÐPb and the ternary AgÐAuÐPb systems are compared with experimental data.
S. Hassam, D. Boa, P. Benigni, J. Rogez, Thermochimica Acta, 510 (2010) 37Ð45
B2565 - Ball-milling and AlB2 addition effects on the hydrogen sorption properties of the CaH2 + MgB2 system
Among the borohydrides proposed for solid state hydrogen storage, Ca(BH4)2 is particularly interesting because of its favourable thermodynamics and relatively cheap price. Composite systems, where other species are present in addition to the borohydride, show some advantages in hydrogen sorption properties with respect to the borohydrides alone, despite a reduction of the theoretical storage capacity. We have investigated the milling time influence on the sorption properties of the CaH2 + MgB2 system from which Ca(BH4)2 and MgH2 can be synthesized by hydrogen absorption process. Manometric and calorimetric measurements showed better kinetics for long time milled samples. We found that the total substitution of MgB2 with AlB2 in the starting material can improve the sorption properties significantly, while the co-existence of both magnesium and aluminum borides in the starting mixture did not cause any improvement. Rietveld refinements of the X-ray powder diffraction spectra were used to confirm the hypothesized reactions.
B. Schiavo, A. Girella, F. Agresti, G. Capurso, C. Milanese, Journal of Alloys and Compounds, 509 (2011) S714ÐS718
B2564 - Thermophysical properties measurement by drop calorimetry and flash method
The methods for precise determination of thermophysical properties are investigated aiming the determination of thermal conductivity through the equation: l = a.Cp.r (thermal diffusivity, heat capacity and density, respectively). The method for heat capacity determination is based on drop calorimetry (Setaram MHTC 1500oC) where a quasi-Calvet type sensor surrounds a crucible and measures the heat flow due to sample drop from ambient up to the cell temperature. Sapphire references were dropped alternatively allowing the determination of the calorimetric constant required for sample drops calculation. The measured enthalpies were fitted as a function of temperature while its derivative gives the Cp = f(T) curve. The flash method for thermal diffusivity determination has been developed by the author*, who has built a diffusivimeter prototype. One special software was written including the transient heat transfer thermal quadrupole theory besides traditional methods, like Parker and temporal moments. The thermal quadrupole is an hybrid analyticalnumerical method where the heat equation is solved in Laplace domain, undergoing later a numerical inversion to real space. The practical result is seen on precision of diffusivity determination, typically into the 1-3% range. The results obtained by drop and flash methods were used to calculate the sample thermal conductivity as a function of temperature.
Thomaz Augusto Guisard Restivo, Bernard Legendre, Thermochimica Acta
B2563 - Enthalpies of mixing of liquid systems for lead-free soldering: CuÐSbÐSn system
Using two different types of high temperature drop calorimeters, partial and integral enthalpies of mixing of liquid alloys were determined in the ternary CuÐSbÐSn system. The system was investigated along four sections at 1100 K. Experimental data were used to find ternary interaction parameters by applying the RedlichÐKisterÐMuggianu model for substitutional solutions, and a full set of parameters describing the concentration dependence of the enthalpy of mixing was derived. From these, the isoenthalpy curves were constructed for 1100 K. The entire system shows exothermic enthalpy of mixing at the given temperature.
Dominika Jendrzejczyk-Handzlik, Meryem Rechchach, Wojciech Gierlotka, Herbert Ipser, Hans Flandorfer, Thermochimica Acta, 512 (2011) 217-224
B2562 - A DSC study of the NaNO3ÐKNO3 system using an innovative encapsulation technique
An innovative encapsulation technique designed for the DSC high temperature measurements of the volatile samples is presented in this study. Stainless steel crucibles with a screwed bolt were developed for this purpose. The technique was demonstrated on the phase diagram measurement of the NaNO3ÐKNO3 system and the obtained results are presented in this study. Up to date two thermodynamic assessments of the NaNO3ÐKNO3 phase diagram have been made, one characterized by a single eutectic point with limited solubilities in the solid state in both NaNO3 and KNO3 rich corners, whereas the other version prefers a continuous solid solubility with minimum on the liquidus line. Based on our results we confirm limited solubilities in the solid state.
O. Bene?, R.J.M. Konings, S. Wurzer, M. Sierig, A. Dockendorf, Thermochimica Acta, 509 (2010) 62Ð66
B2561 - The determination of the integral enthalpies of mixing of liquid AuÐInÐSn alloys and the enthalpy of formation of the Au4In3Sn3 compound
With a view to modelling the AuÐInÐSn alloy system, the enthalpies of mixing of liquid AuÐInÐSn alloys have been measured as a function of Au content by drop calorimetry at 609 ¡C for constant In:Sn ratios of 1:1, 1:3 and 3:1. For each of the three sections studied, the enthalpies of mixing were exothermic. In addition, the enthalpy of formation of the ternary Au4In3Sn3 at 298 K was measured both by direct-reaction calorimetry and by tin-solution calorimetry
A. Watson, G. Borzone, N.Parodi, G. Cacciamani, Thermochimica Acta, 510 (2010) 24Ð31
B2560 - Thermodynamics of the Al3Ni phase and revision of the AlÐNi system
The heat capacity of the Al3Ni phase had been measured for the first time, by means of relaxation method over the low temperature range 2Ð323 K and by measuring heat content increments using drop calorimetry over the higher temperature range of 583Ð1073 K. The Debye function was employed to fit the low-temperature heat capacities, and from the function, the absolute entropy was evaluated, . A three-term polynomial representation, a + báT + cáT?2, was used for describing heat capacity above 298.15 K. The Gibbs energy function of the Al3Ni phase was derived with a fixed reference state by incorporating the polynomial expression of the heat capacity, the recently reported enthalpy of formation and the related phase equilibria in the AlÐNi system. A revised thermodynamic description of the entire AlÐNi system together with the calculated phase diagram is also presented.
H.-L. Chen, E. Doernberg, P. Svoboda, R. Schmid-Fetzer, Thermochimica Acta, 512 (2011) 189Ð195
B2559 - Thermodynamic properties of liquid silverÐgallium alloys determined from e.m.f. and calorimetric measurements
The thermodynamic properties of the liquid AgÐGa alloys were determined using e.m.f. and calorimetric methods. In the e.m.f. method, solid oxide galvanic cells were used with zirconia electrolyte. At first, the Gibbs free energy of formation of pure solid gallium oxide, Ga2O3, from pure elements was derived. Using values of the measured e.m.f. for the cell with xGa = 1.0, the following temperature dependence was obtained. Next, the activity of the gallium was derived as a function of the alloy composition from the values of the measured e.m.f. Activities of silver were calculated using the GibbsÐDuhem equation. The drop calorimetric measurements were carried out at two temperatures, viz. 923 K and 1123 K, using a Setaram MHTC calorimeter. Integral enthalpies of mixing of liquid binary alloys were determined at those temperatures. Finally, thermodynamic properties of the liquid alloys were described with the RedlichÐKister equation using ThermoCalc software.
Dominika Jendrzejczyk-Handzlika, Krzysztof Fitzner, The Journal of Chemical Thermodynamics, 43, 3 (2011) 392Ð398
B2558 - Physicochemical investigation of platinum dichloride polymorphism
The physicochemical characteristics of phase transitions of PtCl2 were investigated for the first time. The irreversible character of the transition from ?-modification to ?-form of PtCl2 and the temperature range of process were established (570Ð870 K). ?-PtCl2 has one reversible transition at a temperature of 660 ± 5 K; the thermal effect of this process is +167 ± 17 J/mol.
Tamara P. Chusova, Zinaida I. Semenova, Thermochimica Acta, 469 (2008) 77-85
B2557 - Kinetics of intermetallic phase formation in the Ti/Al multilayers
The kinetics of the synthesis of elemental nanoscaled multilayers of Ti and Al in the regime of continuous heating from 300 K up to 973 K was investigated. A series of sputter deposited Ti/Al multilayer thin films with individual layer thickness (d) from 4 nm up to 1000 nm have been used. Differential scanning calorimetry, FriedmanÐGupta, Kissinger and Suri-ach methods of complex kinetic analysis, classical and time resolved X-ray diffraction and scanning electron microscopy have been applied. In the Ti/Al multilayers the sequence of reactions leading to the final product TiAl (and Ti3Al) is determined. The final products as well as the kinetics of their formation depend on the individual layer thickness. Three different kinetic regimes depending on the layer thicknesses have been found.
Em'lia Illekov, Jean-Claude Gachon, Alex Rogachev, Hamazasp Grigoryan, Julius Clemens Schuster, Anton Nosyrev, Petr Tsygankov, Thermochimica Acta, 469 (2008) 77-85
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