In this paper, the electrochemical properties and performances of all-solid-state lithium polymer batteries (LPBs) using standard PEO-based solid-state polymer electrolytes (SPEs) are reported and discussed. The assembled cell showed stable charge-discharge cycles (>150 cycles) at 30 C. This is due to desirable solid electrolyte interface (SEI) film formation at the SPE | cathode interface at the first cycle indicated by activation energy measurements for interfacial Li ion exchange reaction. However, sudden capacity fading for prolonged electrochemical cycles was indicated by an accelerated aging test at higher current density (1 C) and temperature conditions (60 C), accompanied by an increase of electrochemical polarization. This degradation phenomenon may be fatal for practical usage of large-scale batteries which requires extremely long-time durability. Two sequential factors affecting the capacity fading are proposed through the studies of in situ 19 F-NMR imaging, real-time monitoring of the total cell thickness, and electrochemical measurements such as AC impedance. One factor is degradation of the cathode sheet or cathode composite assembly, owing to cyclic volumetric change from the two-phase LiFePO 4 -FePO 4 reaction. Such degradation leads to uneven electric contact at the electrode | electrolyte interface, thereby enhancing local electrochemical polarization. The second factor, namely, Li salt decomposition, is triggered by this local polarization, giving rise to the continuous capacity fading and the increase of polarization. This degradation scenario can be general enough to include the full range of all-solid-state LPB devices, since the trigger of degradation owes to non-fluidity of solid | solid contact, or solid electrolytes cannot immerse into the cavities caused by pulverization of cathode particles unlike liquid electrolytes. On the basis of these results, we attempted to improve the mechanical properties of the binder materials of cathode sheets, and demonstrated improved cyclic durability.

Solid‐state lithium polymer secondary batteries (LPB) are fabricated with a two‐electrode‐type cell construction of Li|solid‐state polymer electrolyte (SPE)|LiFePO4. Plasticizers of poly(ethylene glycol) (PEG)‐borate ester (B‐PEG) or PEG‐aluminate ester (Al‐PEG) are added into lithium‐conducting SPEs in order to enhance their ionic conductivity, and lithium bis‐trifluoromethansulfonimide (LiTFSI) is used as the lithium salt. An improvement of the electrochemical properties is observed upon addition of the plasticizers at an operation temperature of 60 °C. However, a decrease of discharge capacities abruptly follows after tens of stable cycles. To understand the origin of the capacity fading, electrochemical impedance techniques, ex‐situ NMR and scanning electron microscopy (SEM)/energy dispersive X‐ray spectroscopy (EDS) techniques are adopted. Alternating current (AC) impedance measurements indicate that the decrease of capacity retention in the LPB is related to a severe increase of the interfacial resistance between the SPE and cathode. In addition, the bulk resistance of the SPE film is observed to accompany the capacity decay. Ex situ NMR studies combined with AC impedance measurements reveal a decrease of Li salt concentration in the SPE film after cycling. Ex situ SEM/EDS observations show an increase of concentration of anions on the electrode surface after cycling. Accordingly, the anions may decompose on the cathode surface, which leads to a reduction of the cycle life of the LPB. The present study suggests that a choice of Li salt and an increase of transference number is crucial for the realization of lithium polymer batteries.

The addition of plasticizers into Li(+)-conductive solid polymer electrolytes (SPEs) is a commonly known technique to enhance the ionic conductivity. Among the used plasticizers, alkoxides of group-13 elements [such as poly(ethylene glycol) (PEG)-borate ester] are promising candidates due to the Lewis acidity of the elements of this group (i.e. B, Al, and so on), which interact with the anions and may increase the degree of dissociation of the salts and the transport number of the SPEs. By means of pulsed-gradient stimulated-echo NMR (PGStE-NMR) and AC impedance measurements, we investigate the effect of Lewis acidity originated from group-13 elements on the transport number and the dissociation rate of SPEs containing various plasticizers. Our results show that the degree of salt dissociation is significantly enhanced by the addition of plasticizers including group-13 elements, whereas only a small or negligible increase of the transport number is observed for these SPEs. We infer that the plasticizers exhibiting Lewis acidity associate with the anions, and that the associated pairs can migrate in the SPEs as fast as free anions, which results in a lower transport number than expected.

The development of a high-frequency, step-tunable gyrotron operating at submillimeter wavelengths is described. The gyrotron design was optimized for operation at the second harmonic of the electron cyclotron frequency in the TE261 cavity mode, whose resonant frequency is 384 GHz. Experimental results show that second harmonic operation can occur without mode competition as long as the beam current is low (Ib ≲0.8 A), but as the current is increased, the fundamental TE231 cavity mode increases and eventually (Ib ≳1 A) suppresses the second harmonic. The competition between the two modes is studied in detail. The starting current for second harmonic operation is also studied experimentally and compared with calculated results. Other resonances have also been examined. With the present superconducting magnet, the maximum frequency achieved is 402 GHz (second harmonic operation in the TE551 cavity mode) at several kilowatts.

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