Baumbach, T.

Kaufholz, M.

Kotapati, S.

Krause, B.

Stüber, M.

Ulrich, S.

English

KITopen

KIT – University of the State of Baden-Württemberg andNational Large-scale Research Center of the Helmholtz AssociationANKA / Institut für Synchrotronstrahlung  (ISS)www.kit.eduIn situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsM.Kaufholz1, B. Krause1, S. Kotapati 1, M.Stüber2, S.Ulrich2 and T. Baumbach1,31 Institut für Synchrotronstrahlung, Karlsruher Institut für Technologie (KIT), 2 Institut für Angewandte Materialien -Angewandte Werkstoffphysik, Karlsruher Institut für Technologie (KIT), 3 ANKA, Karlsruher Institut für Technologie (KIT) Institut für Synchrotronstrahlung (ISS)2 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsContentMotivationIn situ X-Ray ReflectivityThree Examples:In situ XRR at different DC PowerIn situ XRR at different Growth TemperaturesInterruption of DepositionSummary & Outlook Institut für Synchrotronstrahlung (ISS)3 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsMotivationVanadium Carbide (VC1-x)Growth of thin films by SputteringHard coating material for toolsdeposition conditions and microstructure formation define mechanical properties Understand growth process depending on sputtering   conditions Investigation needs suitable methodsnondestructive monitoring of growth process resolution in sub-nanometer scalecompatibility with the gas atmosphereinvestigation of polycrystalline material high deposition rates (0.22 nm/s @ DC Power 200 W)In situ X-Ray ReflectivityInstitut für Synchrotronstrahlung (ISS)4 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsBasics of X-Ray ReflectivitySiVC1-xElectron density (‘Critical Angle’)Thickness (‘Kiessig fringes’)Roughness (‘Slope’) [1]Description by Parratt-Algorithm [2]Fully dynamical description of XRRTwo options to measure in situ XRR1. Full angular range XRR2. XRR at a fixed angular position i f[1] Pietsch, Holy, Baumbach, High Resolution X-Ray Scattering from thin films and lateral Nanostructures, Springer 2004[4] Parratt, Phys. Rev. 95, 2, p. 359-369,(1954)Institut für Synchrotronstrahlung (ISS)5 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsExperimental SetupSetup @ MPI-Beamline:Energy: 10 keVBeamsize: 300OpticsResolution in qz: ~ 0.005 Å-1Detector: Pilatus 1KResolution in time: ~1.1-2.3 sSputter conditions [1]: Target: VC1-x Substrate: Si(100) with natural oxideTarget-substrate Distance: 10 cmArgon Pressure: 2 x 10-3 mbarDeposition rate 0.22 nm/s@ 200 W -2 0 2 4 6-2-1012Specular Beam[1] Krause , Kaufholz et al., J. Synchrotron Rad. (2012),19, 216-222Institut für Synchrotronstrahlung (ISS)6 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsIn situ X-Ray Reflectivity: “full angular range“SiVC1-xHigh deposition rate of 0.22 nm @ 200 W  ~90nm deposition/XRRPossible electron density and roughness changesInterpretation of XRR curve difficultMeasure full angular range i fInstitut für Synchrotronstrahlung (ISS)7 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 100 200 300 400 500 60000.10.20.30.40.50.60.70.80.91x 10-4Time [s.]Intensity [a.u.]1 sDetector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  i fInstitut für Synchrotronstrahlung (ISS)8 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 100 200 300 400 500 60000.10.20.30.40.50.60.70.80.91x 10-4Time [s.]Intensity [a.u.]1 sDetector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  i f20 40 60 80 10000.20.40.60.81x 10-4Time [s.]R [a.u.]Institut für Synchrotronstrahlung (ISS)9 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 100 200 300 400 500 60000.10.20.30.40.50.60.70.80.91x 10-4Time [s.]Intensity [a.u.]1 sDetector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  i fInstitut für Synchrotronstrahlung (ISS)10 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsi fi fDetector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  1 s1 1.2 1.4 1.6 1.8 2 2.210-810-610-410-2100102Intensity [a.u.]i [°]30 s400 sInstitut für Synchrotronstrahlung (ISS)11 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 100 200 300 400 500 60000.10.20.30.40.50.60.70.80.91x 10-4Time [s.]Intensity [a.u.]Detector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  i fi f1 sInstitut für Synchrotronstrahlung (ISS)12 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 100 200 300 400 500 60000.10.20.30.40.50.60.70.80.91x 10-4Time [s.]Intensity [a.u.]Detector and sample are at a fixed angular positionMeasuring Pre- and Post-growth full angular range XRRIn situ X-Ray Reflectivity: “fixed angular position”SiVC1-xSimulation Input: DC Power: 200 W  Deposition Rate:  0.217 nm/s  i fi f3 sInstitut für Synchrotronstrahlung (ISS)13 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsExample 1: Determination of Deposition Rate depending on DC Power at RTIncrease of DC Power by 	 every 250s  	Error due to changes in electron density <1%Sensitive to deposition rate Deposition Rate  ~ DC Power0 200 400 600 800 1000 1200 1400 1600 18002x 104Time [s]5010015020075 W 100 W 120 W 150 W 175 W 200 W50 WIntensity [a.u.]DC Power 50 100 150 20000.10.20.310203040DC Power [W]Deposition Rate [nm/s]Period of Oscillation [s]Institut für Synchrotronstrahlung (ISS)14 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films4Intensity [a.u.]Time [s]600 700 800 900 1000 110005x 10-5σ  =0.3nmσ  =0.4nmExample 2: Monitoring of Roughnessdepending on Growth TemperatureExperiment    SimulationEx situ: AFM 50 100 150 200 250 300 3500,30,40,50,60,70,8 1800 s Deposition timeRoughness(nm)Deposition Temperature °CIncrease of Temperatureleads to increase ofRoughnessConsistent with ex situ AFM600 700 800 900 1000 11000.511.522.53x 10Intensity [a.u.]4T=125°T=451°Institut für Synchrotronstrahlung (ISS)15 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin films0 50 100 150 200 25000.010.020.030.0405101520Time [s]Intensity [a.u.]pressure [mbar]0 1 2 3 4 510010210410610810101 1.1 1.2 1.3 1.4 1.5104105106Intensity [a.u.]i [°]Intensity [a.u.]i [°]Intensity [a.u.]i [°]Interruption of deposition after 200s @ RT and DC Power of 200 W Start depositionXRR after 2. deposition:SiVC1-xExample 3: Different Electron Densities due to Interruption of Deposition11. deposition2. depositionMultilayer of one materialInstitut für Synchrotronstrahlung (ISS)16 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsSummaryIn situ X-Ray Reflectivity is suitable for investigation of VC1-xSensitive to  Deposition Rate Roughness DensitySensitive to different sputtering conditionsOutlookSimulation of in situ XRR curvesGrowth Model (Scaling law)Include diffuse scattering  Limits of methodCombining with other methods for a better understandingIn situ & ex situ X-Ray Diffraction and Absorption Spectroscopy XPS, AFM, TEM, … (in UHV conditions)Measuring Hardness via Nano-/MicroindentationInstitut für Synchrotronstrahlung (ISS)17 29.03.2012 DPG- Frühjahrstagung Berlin 2012, M. Kaufholz In situ X-Ray Reflectivity measurements during Sputtering of Vanadium Carbide thin filmsAcknowledgementsM. Mantilla for technical support @ MPI Beamline @ ANKAH. Gräfe for technical support @ UHVLab @ ANKAS. Darma, J. Gemmler for fruitful discussionFinanced in the framework of Excellence Initiative within the project KIT-Nanolab@ ANKA  Thank You for Your Attention !

In-stiu X-ray reflectivity measurements during DC sputtering of vanadium carbide thin films

https://publikationen.bibliothek.kit.edu/230090542/3816253

In-stiu X-ray reflectivity measurements during DC sputtering of vanadium carbide thin films

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