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High-temperatures in-situ XRD studies of CrN and TiN films

High-temperatures in-situ XRD studies of CrN and TiN films. Experimental: XRD at high T XRD patterns, lattice parameter evolution and grain growth of CrN films XRD patterns, lattice parameter evolution and grain growth of TiN films

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High-temperatures in-situ XRD studies of CrN and TiN films

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  1. High-temperatures in-situ XRD studies of CrN and TiN films • Experimental: XRD at high T • XRD patterns, lattice parameter evolution and grain growth of CrN films • XRD patterns, lattice parameter evolution and grain growth of TiN films • XRD patterns, lattice parameter evolution and grain growth of CrN and TiN films after the optimization of the HV system

  2. X-RAY GAS PUMP Xpert Philips diffractometer: HV apparatus • Optimization • Baking (heating sequence); • Helium streams. 5•10-5 mbar 1•10-5 mbar 1•10-6 mbar 5•10-6 mbar 1•10-7 mbar 6•10-7 mbar

  3. Experiment 1 1000°C 900°C 800°C 700°C 600°C 500°C 5 min - 20°C/min 400°C 35 min 5 min RT RT Deposition PVD Substrate WC Thickness 5 - 10 m XRD Temperature RT - 1000°C Pressure 5.6•10-5 - 1.2•10-4 mbar

  4. CrxN1-x phase diagram

  5. CrN Experiment 1

  6. Optical images Prior to measurements After measurements

  7. UnitCell Grain growth (Scherrer formula)

  8. TixN1-x phase diagram  =Ti - hcp  =Ti - bcc • =TiN  =Ti2N ‘=Ti2N

  9. TiN Experiment 1

  10. Optical images Prior to measurements After measurements Lattice parameter Grain growth

  11. 1000°C 900°C 800°C 700°C 600°C 500°C 5 min - 20°C/min 400°C 35 min 200°C 1 hour RT RT Experiment 2 XRD Temperature RT - 1000°C Pressure 1.7 - 7.7 •10-5 mbar He streams Baking at 200°C for 1 hour 5 min

  12. CrN Experiment 2

  13. Temperature dependence of lattice parameter and grain size Experiment 2

  14. TiN Experiment 2

  15. Temperature dependence of lattice parameter and grain size Experiment 2

  16. Performed measurements and upgrading • Optimization of Vacuum system - XRD at various temperatures on CrN and TiN films • Temperature dependence of lattice parameters • Temperature dependence of grain sizes

  17. Conclusions • CrxN1-x films exhibit phase stability in the cubic CrN form up to • 800°C at actual measurement conditions • After 800°C the CrxN1-x samples undergo to oxidation and the • formation of Cr2N • All TixN1-x films exhibit the presence of the cubic TiN phase and • traces of the Ti2N phase • After 800°C the CrxN1-x samples undergo to oxidation • at actual measurement conditions • After 800°C the TixN1-x samples undergo the formation of Cr2N; • In general the high temperatures result in an increase of the lattice • parameters • In general, the temperature dependence of grain sizes exhibit an • upward trend

  18. Next Studies • Further optimization of vacuum system • Control of pO2 to perform reproducible measurements • - Kinetic and thermodynamic studies • Composition (EDX) • Phase content quantification (XRD) • XPS studies • Morphology study (SEM) • Texture evolution study (XRD) • Mechanical properties • Stress study using XRD (TEC, oxidation, phase • transitions, etc)

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