Characterisation of Ti-6Al-4V/glass-ceramic and pre-oxidised Kovar/glass-ceramic interfaces.

摘要

Glass-to-metal seals are used in a wide range of components. The nature of the interfaces between the constituents is often crucial to the performance of the seal and thus the aim of this study was to characterise the various interfaces in a novel seal made from a strontium boroaluminate glass-ceramic and the alloys Ti-6Al-4V and Kovar (Fe-29Ni-17Co). A titanium boride was found, by STEM, EELS and WDX, to have formed at the glass-ceramic to Ti-6Al-4V interface and to be bonded to both the metal on one side and the glass-ceramic on the other, in contrast to the classic view of glass to metal interfaces where bonding is thought to be promoted through metal dissolving into the glass / glass-ceramic. To establish bonding at the other interface, it was necessary to grow an oxide layer on the Kovar, by heating in air at 700 °C or 800 °C for 10 minutes. The oxide grown at both temperatures was shown (by XPS, XRD, SEM, EDX, STEM and Raman) to have the same composition, with the only significant difference being thickness (2.1 +/- 0.6) µm and (4.0 +/- 0.2) µm thick, for the oxides grown at 700 °C and 800 °C respectively. However, the oxide was found to be much more complex than was indicated by prior literature, comprising four layers. The top layer of the oxide was (Fe,Co)_3O_4, with an Fe_2O_3 layer beneath it. Below these layers were a further two layers of (Fe,Co,Ni)_3O_4. When heated to 800 °C, to simulate the sealing conditions, the oxide was changed to an Fe_3O_4 layer with metallic cobalt and nickel inclusions. Bonding was shown, by SEM and STEM, to occur between the oxidised Kovar and the glass-ceramic, as a result of dissolution of iron from the oxide into the glass. Although the interfaces were not definitively optimised, the seals produced were satisfactory and hermetic.