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

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Presentation transcript:

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

PUMP GAS X-RAY mbar mbar mbar Optimization Baking (heating sequence); Helium streams mbar mbar mbar Xpert Philips diffractometer: HV apparatus

Deposition PVD SubstrateWC Thickness  m XRD TemperatureRT °C Pressure mbar Experiment 1 RT 400°C 500°C 600°C 700°C 800°C 900°C 1000°C RT 35 min 5 min - 20°C/min 5 min

Cr x N 1-x phase diagram

CrN Experiment 1

Optical images Prior to measurements After measurements

UnitCell Grain growth (Scherrer formula)

 =Ti - hcp  =Ti - bcc  =TiN  =Ti 2 N  ‘=Ti 2 N Ti x N 1-x phase diagram

TiN Experiment 1

Optical images Prior to measurements After measurements Lattice parameterGrain growth

Experiment 2 XRD TemperatureRT °C Pressure mbar He streams Baking at 200°C for 1 hour RT 400°C 500°C 600°C 700°C 800°C 900°C 1000°C 200°C RT 35 min 5 min - 20°C/min 1 hour 5 min

CrN Experiment 2

Temperature dependence of lattice parameter and grain size Experiment 2

TiN

Temperature dependence of lattice parameter and grain size Experiment 2

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

Conclusions - Cr x N 1-x films exhibit phase stability in the cubic CrN form up to 800°C at actual measurement conditions 800°C at actual measurement conditions - After 800°C the Cr x N 1-x samples undergo to oxidation and the formation of Cr 2 N formation of Cr 2 N - All Ti x N 1-x films exhibit the presence of the cubic TiN phase and traces of the  Ti 2 N phase traces of the  Ti 2 N phase - After 800°C the Cr x N 1-x samples undergo to oxidation at actual measurement conditions at actual measurement conditions - After 800°C the Ti x N 1-x samples undergo the formation of Cr 2 N; - In general the high temperatures result in an increase of the lattice parameters parameters - In general, the temperature dependence of grain sizes exhibit an upward trend upward trend

Next Studies - Further optimization of vacuum system - Control of pO 2 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) transitions, etc)