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1 Dr. Stefan Schlichtherle Dr. Georg Strauss PhysTech Coating Technology GmbH Decorative vacuum coating technologies 30.05.2014 Certottica Longarone Thin Film Plasma Coating Technologies
2 Content The fascination of functional surfaces produced by thin film technology Presentation of PhysTech Typical applications and examples Functional surfaces PVD (Physical Vapour Deposition) technology Some realised examples
3 PhysTech
4 Thin Film Technology Functionalising of surfaces by PVD technologies Thin films produced by PVD technologies can show a lot of specific properties from nm to m they make tools hard and wear resistant they transmit, reflect or filter light they protect and decorate surfaces they isolate against heat or coldness they improve electric conductivity they realise diffusion barriers
5 Thin Film Technology Tribology Optics Surface protection Tools Medical Implantats Electronics ...
6 PVD technology Coating material transfer mechanisms Three fundamental mechanisms Evaporation Sputtering Exploding Plasma Ablation E-gun for evaporation magnetron plasma arc source deposition
7 PVD technology Evaporation Sputtering Transport of particles Condensation - Ablation in the plasma Bias working gas, e.g. Ar electrons Ions +/- atoms molecules reactive gas, e.g. O2, N2 radicals Starting material: Targets, cathodes, granulate, Gas phase: Substrate: ingots, tabs Plasma Glass, metal, plastic
8 PVD technology solid liquid gaseous plasma energy/temperature gas molecules gas molecules excited Ions molecule fragments free electrons highly excited
9 PVD technology Different plasmas in pvd technologies
10 PVD technology Balzers/Evatec BAP 800 Leybold APS 900/1100 Optical Interference Coatings, N. Kaiser, H.K. Pulker, (Eds.), Springer, 2003
11 PVD technology Balanced magnetron configuration Unbalanced magnetron configuration Characteristics of Sputtering Sputtering variants Sputter Threshold dc magnetron sputtering Sputter Yield dc pulsed magnetron sputtering Sputter Rate rf sputtering Non reactive reactive process dual beam sputtering ion beam sputtering closed field sputtering
12 PVD technology Scematic of a magnetron sputter process
13 PVD technology Different voltage configuration in DC-PMS
14 PVD technology Electrical schematic of a pulse generator AE Pinnacle Plus 5kW: 0-350kHz pulse generator
15 PVD technology 1 substrate holder 4 gas inlet system 2 arc sources - cathodes 5 gas inlet system 3 vacumm pumping system 6 substrates, products
16 PVD technology
17 PVD technology Macroparticle filter, LBNL, Berkeley Particle separation with magnetic systems (Droplets, Makropartikel)
18 PVD process analysis Plasmamonitorsystem PPM421 (Inficon) differential pumped mass spectrometer with additional energy analyser (CMA) detection of ions and neutrals measurement of the ion energy distribution of the relevant process ions detection unit: SEV pressure range: up to 10-1 mbar
19 PVD process analysis Langmuir Probe System an electrical conductable and (Scientific Instruments) heatable electrode is inserted into the plasma measurement of the voltage- acquisition current characteristic and electronics calculation of plasma parameters gabing electronics for as particle densities, electrical boxcar mode (100 kHz) potentials and ion currents trigger relative simple configuration langmuir probe Plasma Principle setup
20 PVD process analysis Ion energy distribution and degree of ionisation Evaporation: Magnetron Sputtering DC Pulsed Sputtering IBAD PLAD, ARC Source DC Pulsed Sputtering
21 PVD process analysis Surface reactions and bombardement effects energetic particle reflected secondary sputtered ions or neutrals electrons atoms or ions adsorbed surface species enhanced chemical reactions surface redeposited backsputtered enhanced surface mobility surface surface region lattice defects trapping collision cascade displacement channeling implanted near surface region Surface: Interface between solid material and gas (vapour or vacuum) Surface region: depth of penetration of the bombarding particles Near surface region: region below depth of penetration, but is also influenced by e.g. Schematic of energetic particles, Heating or diffusion which bombard the growing film Bulk region: region were the material is not (bombardement) influenced by the bombarding effects
22 PVD process analysis Surface reactions and bombardement effects The effects of bombardment of In the subsurface region energetic species (ions, neutrals) on the impinging particles may the surface and the surface region be physically implanted include: the collision cascades cause desorption of weakly bonded surface displacement of atoms and species the creation of lattice defects ejection of secondary electrons surface species may be reflection of the energetic species as recoil-implanted into the high energetic neutrals surface lattice sputter ejection of surface atoms by mobile species may be momentum transfer through collision trapped at lattice defects cascades particle kinetic energy is sputtering and re-deposition of mostly converted into heat sputtered species enhanced mobility of surface atoms enhanced chemical reaction of impinging and adsorbed species.
23 PVD process analysis Ti+ ions dc Process parameters: 5 10 Distance to Ti target: 20cm 50kHz Pulse frequency: 50kHz - 250kHz 100kHz Pulse width: 1296ns 250kHz I=0,5A -3 -3 4 ptot=3,4*10 mbar - 5*10 mbar 10 Pel=67W - 162W cps flow Ar =210sccm flow N2 =30sccm 3 10 2 10 0 20 40 60 80 100 energy in eV Ion energy distribution in a TiN DC-pulsed Magnetron process
24 PVD process analysis 7 10 Ti+ ions Process parameters: Iarc=85A Arc target Ti (distance=20cm) 6 PN2 variable 10 -3 ptot=1*10 mbar -2 ptot=1*10 mbar -1 5 10 ptot=1*10 mbar cps 4 10 3 10 2 10 0 20 40 60 80 100 120 energy in eV Ion energy distribution in a TiN Arc Source process
25 PVD process analysis Power Ekin of Beam Deposition Current density on particles velocity rate density on target substrate e-gun 2 104 Wcmmet < 0,3 eV 103 m s 1 High evaporation 2 103 Wcmdiel Reactive Low Voltage Ion > 104 Wcm 2 15 60 eV High 0, 2 1 mAcm 2 Plating Magnetron 1 15 eV > 10 Wcm 2 Medium 0,1 mAcm 2 sputtering Ion beam 5 100 eV > 10 Wcm 2 104 m s 1 Low Medium 0,5 1 mAcm 2 sputtering Pulsed laser 107 1010 Wcm 2 10 100 eV 104 m s 1 High > 1 mAcm 2 ablation Arc source 107 1010 Wcm 2 20 100 eV 104 m s 1 High > 1 mAcm 2 ablation
26 PVD film growth
27 PVD film properties Einstellung von Schichteigenschaften Stoichiometry Adherence Purity Hardness Structure Abrasion Microstructure resistance Homogeneity Stress Isotropy Topography Density Anforderungen an optische Schichten: Abhngigkeit der Dichte abhngigen Reproduzierbare und stabile Brechungsindexe Eigenschaften von der kinetischen Energie der bombardierenden Teilchen fr verschiedene Geringe optische Verluste Prozesstechnologien Oberflchenschutz vor Flssigkeiten, Gasen, Festkrperteilchen, Strahlung
28 PVD process technologies Correlation: process parameters plasma properties - film properties Process parameter: process pressure, target material, target power density, applied currents and voltages, pulse frequency and duty cycle Plasma properties: Kinetic energy of ions Ion current density Film properties: Density and morphology of films Oxide films Nitride films for optical applications for tribological and tool applications Refractive index Adhesion Mechanical stress Mechanical stress Optical loss Hardness
29 PVD technology Arc Source Deposition (PhysTech)
30 PVD technology Magnetron Sputter Coater (Edwards)
31 PVD technology Gas-Flow-Sputtering (PhysTech)
32 Research activities EMPA Dbendorf (CH) CeTeV Carsoli (I)
33 Research activities IonBond Newcastle (GB)
34 Thank you for your attention
35 Typical applications Magnetron sputter plasma for the Activation of plastic parts deposition of optical thin films HIPIMS High Plasma Impuls Magnetron Sputtering Filtered Arc Source Deposition of tribological and hard coatings Deposition of hard coatings
36 Typical applications Arc Source Deposition Corrosion protection by Innova - Balzers atmospheric plasma Arc Source Tools Tribology Surface protection deposition Plasma atmospheric plasma deposition increases the polarity of the plastic surface increased adhesion Cleaning of metal parts by plasma pre-treatments
37 Typical applications Plasmapolymerisation treatment of temperature sensitive parts and realisation of specific surface properties like anti-finger-printing, easy to clean, anti-adhesion Pulsed magnetron sputtering Decorative hard coatings, z.B. TiN, for architectual glass coating TiAlN, CrN
38 Typical applications Ion beam assisted deposition for deposition of APS advanced plasma source High precision optical interference coatings Deposition of optical multilayer systems
39 Typical applications Plasmanitrieren: Plasma nitriding is a thermo-chemical process to modify surfaces and barrier layers. It is based on the incorporation of nitrogen into the surface of the component. Process gases are: ammonia, nitrogen, methane and hydrogen. Plasma nitriding takes place in a vacuum chamber under ionic gas atmosphere. To produce wear resistant films sometimes a mixed gas atmosphere is used. The quality of the nitrided surface is dependent on the gas mixture, pressure, temperature and process time. Applications: tools, mechanical components, winds, engine parts like crank shafts, camshafts or valves
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