Page 19 - Shimadzu Journal vol.10 Issue1
P. 19

Materials Science









               Note that since thermal conductivity
            is different  between  argon and air, the
            heat  exhaust  mechanism  of  the  instru-
            ment may not function properly, thereby
            preventing acquisition of correct infrared
            spectra. To avoid this, we used a cooler to
            enhance heat exhaustion in this analysis,
            and controlled the dew point in the glove
            box to -70 ˚C (moisture content of 2.58
            ppm) or lower, and the oxygen concen-
            tration to 0.3 ppm or lower. Analysis in
            a glove box thus enables highly accurate
            measurements without being affected by   Fig. 2 Example of IRSpirit Glove   Fig. 3 IRSpirit (Left) and Wireless Converter (Right) in Glove Box
            water vapor or oxygen.            Box System





                    Effect of Atmospheric Gases on
                Measurement of Electrolyte Solutions for
                    Lithium-Ion Secondary Batteries
                                                                                                  Argon atmosphere
            An  electrolyte  of  EC  (ethylene  carbonate)  +  DEC  (diethyl  car-
            bonate) (3 : 7) solution containing 1M LiPF (lithium hexafluoro-
                                           6
            phosphate), an organic  electrolyte  solution commonly  used in
            lithium-ion secondary batteries, was measured under air and argon
            atmospheres. Fig. 4 shows the measured infrared spectra and Fig. 5                     Air atmosphere
            shows the enlarged region between 2800 and 4000 cm  in Fig. 4.
                                                 -1
               Although the optical properties of argon and air are very dif-
            ferent, Fig. 4 shows that the infrared spectra acquired under both   Fig. 4 Infrared Spectra of EC+DEC (3 : 7) Electrolyte Solution Containing
                                                                 1M LiPF
            atmospheres were almost identical, appearing to be unaffected by   6
            the difference of atmosphere.
               Note that in Fig. 5, the broad absorption of symmetric and an-
            tisymmetric OH-stretching vibrations from water molecules were
            observed between 3400 and 3700 cm  under the air atmosphere.                          Argon atmosphere
                                      -1
            Meanwhile, the influence was negligible in the infrared spectrum
            under the argon atmosphere.
                                                                                 Symmetric OH-stretching
                                                                                 vibration
                                                                                 Antisymmetric OH-stretching
                                                                                 vibration         Air atmosphere
                  Measurement of Electrolyte Solution
                   for Lithium-Ion Secondary Battery             Fig. 5 Infrared Spectra of EC+DEC (3 : 7) Electrolyte Solution Containing
                          in Inert Atmosphere                    1M LiPF (Enlarged)
                                                                      6
            Organic electrolyte solutions are used as the electrolyte solution
            for lithium-ion secondary batteries, and their moisture content
            is strictly controlled. Such an electrolyte solution was measured
            by FTIR in an argon atmosphere.
               Fig. 6 shows the infrared spectra of EC+DEC (3 : 7) electrolyte
            solution with 1M LiPF  and EC+DEC (3 : 7) solution without 1M
                            6
            LiPF . The only difference between the two samples is the presence
                6
            or absence of LiPF .
                         6
            * In this application, measurements were performed under specific conditions
            and environments since glove boxes and argon atmospheres reduce the heat
            exhaust function and may prevent proper instrument operation. Please contact
            for details.                                         Fig. 6 Infrared Spectra of EC+DEC (3 : 7) Electrolyte Solution Containing
                                                                 1M LiPF  (red) and EC+DEC (3 : 7) Solution (black)
                                                                      6



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