Repetition: Adhesion Mechanisms

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1 Repetition: Adhesion Mechanisms a) Mechanical interlocking b) Monolayer/monolayer c) Chemical bonding d) Diffusion e) Psedo diffusion due to augmented energy input (hyperthermal particles)

2 Repetition: Adhesion Measurement a) Substrate b) Coating c) Glued stud Attention: the following ucertainties may be present: + Reaction coating/glue + Diffusion of glue into coating + After diffusion: reaction glue/ substrate + Lack of adhesion glue/coating

3 Repetition: Structure Zone Models Growth phases of a coating Nucleation on substrate Partial coalescence and interface formation Total coalescence and polycrystal formation Growth of polycrystal grains Structure zone models yield a qualitative image of film growth, morphology and crystallography in dependence on the coating parameters.

4 Repetition: Growth Mechanisms Zone Mechanism Char. feature 1: T/T M <0,2 T: T/T M <0,4 2: T/T M <0,8 3: T/T M >0,8 Shadowing Particle energy Surface diffusion Volume diffusion Fibers, pores Nano grains Columnar crystlites 3d - Grains

5 Repetition : Thickness Measurement I d = m ρ S A d = Thickness ρ S = Density A = Substrate surface Attention: The coating density, ρ S, is in most cases different from the bulk density, ρ D.

6 Repetition : Thickness Measurement II Prinziple: Two beam interference Example: Multiple coating Optical thickness: λ λ n d = n Optical d Re al

7 Friction and Wear Friction: No removal of material F=µFg r F=mg g F g µ = Friction coefficient 0 < µ < 4-5(!); µ is not confined to values smaller 1 F g F g F = µ F r No dependence on the extension of the interacting surfaces! =>microscopic interaction unclear! n Wear: Removal of material associated with weight loss

8 Friction and Wear: Measurement Friction: + Linear load (scratch-test) + Pin on disc + Disc on disc + Special tribometers Wear: + All above methods with analysis of transfer films and abraded coatings + Abrasion measurement by thickness control + Slurry-abrasion + Special test rigs

9 Micro Hardness Defined by the residual deformation of a material due to the penetration of an (ideally) undeformable test body. Test body material: + Diamond Test body geometries: + Vickers: Pyramid with diagonal vs. height 1:7 + Knoop: three sided pyramid + Rockwell: sphere + Wedge Test loads: N

10 Micro Hardness: Test Geometry Ultra micro hardness-tester, Vickers geometry: Test body a) Strain gage b) Sample c) Double spring d) Coil e) Clutch f) Base plate Micro hardness impressions This type of hardness tester can easily be implemented into an optical or a scanning electron microscope.

11 Nanoindenter The Nanoindenter also allows the determination of the elastic (reversible) deformation (i. e. of the elastic modulus) of the sample. Force Elastic modulus load unload In the case of coatings care has to be taken that the indentation depth of the test body is less than 1/3 of the film thickness. Only under this condition the influence of the substrate can be neglected. Residual deformation Penetration depth

12 Non-Destructive Hardness Measurement Hertzian contact: Point force acting onto an ideally elastic half-plain: z F w(r)=f(f,g, ν) w(r) corresponds to the indentation depth of the test body. G and ν result from the elastic constants of the sample: G = c 44 0 w(r) G...Shear modulus ν...poisson ratio r ν= c12 2( c + c ) 44 12

13 Determination of Elastic Constants Elastic constants can be determined by the measurement of the sound velocity of longitudinal und transversal vibrational modes wthin a solid body.

14 Surface Acoustic Waves Exciatation of longitudinal and transversal surface modes by a defined laser pulse: Piezoelectr. transducer Laser pulse at time t 0 Surface wave package From the runtime of the wave package the sound velocity can be determined. From this the elastic constants can be deduced. The excitation of surface waves allows the application of this principle to thin films.

15 Hardness: Important Influences The follwing material parameters may influence hardness: + Sress state + Temperature + Grain size + Impurities + Degree of deformation

16 Mechanical Properties: Spatial Resolution By Scanning Force Microscopy the following mechanical (surface) properties can be determined spatially resolved on the nanometer scale: + Elastic modulus + Hardness + Adhesion strength This is possible by the so-called force spectroscopy

17 Force-Distance curves: a/b: Approach b/c: Snap-on c/d: Repulsive region d/f: Pull-back e: Zero transient f/g: Detatchment of tip g/h: Force free pull-back

18 Pulsed Force Mode Repated recording of force/distance curves during an AFM-scan with electronic analysis: Force-distance curve: Polymer chains: Topography free cantilever oscillation Adhesion Stiffness

19 Artifacts Important artifact of force spectroscopy: Formation of a water meniscus between tip and surface under regular envronmental conditions. AFM-tip Water meniscus The meniscus primarily modifies the values for the adhesion of the tip to the surface due to the high surface tension of water. Preventive measures: + Work under dry nitrogen + Work in liquids + Work under inert gas + Work under HV

20 Ductility Bulk material: breaking strain ε b [%] ε B = lz l l 0 0 l Z = Sample length at breaking point l 0 = Length of uncharged sample ε B = Breaking strain [%] Thin film: 3-point-bending test Cracks ε B 100d 2R + d d = Film thickness R = Radius of curvature for first crack formation

21 Stresses Kinds of stress: σ = σ + σ + σ MECH T I Mechanical Stress: σ MECH Can be triggered by clamping the substrate and subsequent relaxation Thermal stress: σ = E ( α α )(T T ) Triggered by different coefficients T S S U B M of thermal expansion (CTE) of E S... Elastic modulus coating substrate and coating α S... CTE, coating α U... CTE. substrate T B... Coating temperature T M... Temperature of stress measurement

22 Stresses and Film Structure Intrinsic stress: σ I Intrinsic stresses are a direct consequence of the coating structure and the deposition conditions. Tensile stress Compressive stress Variable Compressive stress Tensile stress

23 Intrinsic Stress: Sputtering

24 Stress Measurement: Fundamentals Curved Substrate: Tensile stress Compressive Stress Total stress σ of a thin film: σ = Esd 6(1 ν 2 s s )d F 1 R s1 1 R s2 a) Substrate b) Coating c) Reference plate E S... Elastic Modulus substrate ν S... Poisson Ratio substrate d S... Substrate thickness d F... Film thickness R S1, R S2... Radius of curvature before/after coating, respectively

25 Stress Measurement: Interference Optics a) Substrate b) Coating c) Reference plate (plane glass) d) Beam divider e) Light source f) to acquisition optics R s = 2 2 Dm Dn 4λ( m n) D M... Diameter m-th Newton-fringe D N... Diameter n-th Newton-fringe λ... Wavelength of incident light

26 Stress Measurement: Geometric Optics a) Coated substrate b) Glass plate with reflecting coating c) Beam divider d) Display e) Image uncoated substrate f) Image coated substrate g) Incident light R = 2yD ' y y + y... Sample diameter y +... Image diameter uncoated sample y'... Image diameter coated sample D... Distance sample/display

27 Stress Measurement: Cantilever Geometry: Principle: α tan(2α) H Substrate Coating Compressive stress Tensile stress l l R S δ α 1 2 a tan H l sin α α = R S R S l 2 a tan H 2lH H 2α Neglections and assumptions: a) no lateral displacement of cantilever b) no vertical displacement of cantilever(δ) c) low /H

28 Stress Measurement: X-Rays Principle: Measurement of the global deformation of the elementary cell by: + Interstitials + Vacancies Advantages: + Non-destructive + In Situ possible Disadvantages: Numerous error sources: + Lattice defects + Dislocations + Impurities + Impurity phases

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