TEM in-situ observation of SiO2 Doped TZP at High Temperatures

Y. Ikuhara, Y. Nagai, T. Yamamoto, T. Sakuma

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1 Citation (Scopus)


Chemical reaction of SiO2 and TZP(Tetragonal Zirconia Polycrystal) was directly observed by using TEM in-situ heating technique in order to understand the behavior of SiO2 to TZP at high temperatures. The dynamic interaction of SiO2 and TZP was recorded up to about 1400°C by the CCD camera-video system which was connected to TEM. It was found that most of SiO2 phase is dissolved into ZrO2 grains at above 1300°C. On the other hand, during cooling from the high temperature to around 400°C, amorphous SiO2 reprecipitated from the surface of ZrO2 grains and formed a thin layer around the ZrO2 grains. This result agrees well with the fact that silicon segregates in the vicinity of the grain boundaries in SiO2-doped TZP. In order to confirm the grain boundary segregation at high temperatures, the grain boundaries in the quenched specimen were investigated by high resolution electron microscopy (HREM), energy dispersive X-ray spectroscopy (EDS) and electron energy loss spectroscopy (EELS). It was found that no amorphous phase was present between two adjacent grains even in the quenched samples. EDS analysis revealed that silicon segregated at the grain boundaries and its width was larger than that in as-sintered specimen. Electron energy loss near edge structure (ELNES) of O-Kedge was measured from both grain boundary and grain interior in the quenched specimen.

Original languageEnglish
Pages (from-to)525-530
Number of pages6
JournalMaterials Science Forum
Publication statusPublished - 1999


  • Electron energy loss spectroscopy (eels)
  • Grain boundary
  • High resolution electron microscopy (hrem)
  • Segregation
  • Tem in-situ observation


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