The state of lithium in a novel hard-carbon optimized to the anode of large size Li ion secondary battery, which has been recently commercialized, was investigated and compared with other existing hard-carbon samples by 7 Li NMR method. The new carbon material showed a peak at 85 ppm with a shoulder signal at 7 ppm at room temperature in static NMR spectrum, and the former shifted to 210 ppm at 180 K. The latter at room temperature was attributed to Li doped in small particles contained in the sample. The new carbon sample showed weaker intensity of cluster-lithium signal than the other hard-carbon samples in NMR, which corresponded to a tendency of less "Constant Voltage" (CV) capacity in charge-discharge curves of electrochemical evaluation. Smaller CV capacity and initial irreversible 2 capacity, which are the features of the novel hard-carbon, are considered to correspond to a blockade of the diffusion of Li into pore of carbon.
The existence of micropores and the change of surface structure in pitch-based hard-carbon in xenon atmosphere were demonstrated using 129 Xe NMR. For high-pressure (4.0 MPa) 129 Xe NMR measurements, the hard-carbon samples in Xe gas showed three peaks at 27, 34 and 210 ppm.The last was attributed to the xenon in micropores (smaller than 1 nm) in hard-carbon particles. The NMR spectrum of a sample evacuated at 773 K and exposed to 0.1 MPa Xe gas at 773 K for 24 h showed two peaks at 29 and 128 ppm, which were attributed respectively to the xenon atoms adsorbed in the large pores (probably mesopores) and micropores of hard-carbon. With increasing annealing time in Xe gas at 773 K, both peaks shifted and merged
The pulpal origin of dentinal immunoglobulins was demonstrated by means of immunohistological methods. Immunoglobulins were located both in the cytoplasm of odontoblasts in pulp and at odontoblastic processes in dentin. Positive reactivity of the immunoglobulins to antigens was confirmed using peroxidase-immunized rabbits. IgG, IgA, IgM, C3, and C4 were observed on some invasive bacteria in human carious dentin.
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