The Influence Of Deposition Temperature On The Zirconia Film Microstructure

ZrO2 has a high melting point, low thermal conductivity, high dielectric constant, high ionic conductivity and high temperature chemical stability, and is widely used in optical films, catalytic films and oxide fuel cell films. ZrO2 has three crystal phases: monoclinic phase (M), tetragonal phase (T) and cubic phase (C). Therefore, ZrO2 will undergo a phase change with temperature changes, resulting in a significant volume effect, and the thermal conductivity of ZrO2 is small, and the thermal expansion coefficient is large, which makes the thermal shock resistance of pure ZrO2 very poor, thus limiting the application of ZrO2. Adding an appropriate amount of oxide stabilizers to ZrO2, such as Y2O3, MgO, and CaO, can stabilize ZrO2 in the high-temperature phase. Among them, Y3+ radius (0.09nm) and Zr4+ radius (0.08nm), Y2O3 refractive index (1.9) and ZrO2 refractive index (2.0) are very close, so the addition of Y2O3 will not cause a significant change in the lattice constant of ZrO2 and the refractive index. Significantly lower, Y2O3 stabilized ZrO2 film (YSZ) exhibits good physical and chemical properties.

Therefore, Y2O3 is used to stabilize ZrO2. The preparation methods of ZrO2 film include magnetron sputtering, pulsed laser deposition, electron beam evaporation, ion beam assisted deposition, etc. Among them, the magnetron sputtering method has high film deposition rate and good bonding performance with the substrate, so it is widely used use. In magnetron sputtering, the sputtering rate of metal targets is several to tens of times higher than that of compound targets. Therefore, metal targets are often used to prepare ZrO2 and YSZ films in practical applications. The temperature of the substrate has a great influence on the structure and surface morphology of the film prepared by reactive sputtering. Therefore, exploring the influence of the deposition temperature on the microstructure of ZrO2 and YSZ films has important application value. In this paper, the DC reactive magnetron sputtering method was used to prepare ZrO2 thin films and yttrium stable oxidation using pure Zr target material (purity 99.999%, mass fraction, the same below) and Y-Zr alloy target material (Y content 14.2mol%). Zirconium film (YSZ), and the influence of substrate deposition temperature (25℃ and 300℃) on the microstructure of ZrO2 film and Y2O3 stabilized ZrO2 film was studied.

The experiment uses the JGP450 multi-target magnetron sputtering apparatus, the substrate is K424 alloy, and the substrate is ultrasonically cleaned in absolute ethanol and acetone for 30 minutes and then dried for use. The background vacuum during coating is 6.6×10-4Pa, the sputtering gas and reaction gas are Ar (purity 99.999%) and O2 (purity 99.999%), the sputtering power is 90W, the sputtering pressure is 1.0Pa, Ar and The O2 flow rate was 30mL/s and 4mL/s, the target base distance was 60mm, the sputtering time was 60min, and the substrate temperature was 25°C and 300°C, respectively. A nickel-chromium-silicon thermocouple is used to control the temperature of the substrate, and it is stable for 30 minutes after reaching the set temperature. Before coating, the target material was pre-sputtered for 20 minutes in a pure Ar atmosphere for cleaning, then O2 was introduced, and the experiment was started after the glow stabilized.

ZrO2 films and YSZ films were prepared by DC reactive magnetron sputtering at 25℃ and 300℃, respectively.

The results show that the deposition rate of ZrO2 films at different deposition temperatures is not much different, while the deposition rate of YSZ films is higher at room temperature, and ZrO2 films are easier to crystallize than YSZ films under the same deposition conditions. The ZrO2 film prepared at 25℃ is amorphous, with only a small amount of crystalline state in the film; the ZrO2 film deposited at 300℃ has obvious crystallinity, the film is a monoclinic structure of polycrystalline, and the crystals grow in free orientation. The YSZ films prepared at 25°C and 300°C are all amorphous. As the deposition temperature increases, the surface of the ZrO2 film tends to be dense and flat, while the surface of the YSZ film becomes rougher.

Please keep the source and address of this article for reprinting:The Influence Of Deposition Temperature On The Zirconia Film Microstructure

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