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Plasma, electron and ion beams surface patterning of metals.
 

Plasma, electron and ion beams surface patterning of metals.

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Apresentado pelo professor Thierry Czerwiec (Institut Jean Lamour, Nancy, France) no dia 12 de junho na Universidade de Caxias do Sul, em seminário realizado pelo Instituto Nacional de Engenharia de ...

Apresentado pelo professor Thierry Czerwiec (Institut Jean Lamour, Nancy, France) no dia 12 de junho na Universidade de Caxias do Sul, em seminário realizado pelo Instituto Nacional de Engenharia de Superfícies e o PGMAT da UCS para um público de 16 estudantes e professores.

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    Plasma, electron and ion beams surface patterning of metals. Plasma, electron and ion beams surface patterning of metals. Presentation Transcript

    • Plasma, electron and ion beams surface patterning of metals T. Czerwiec, G. Marcos Institut Jean Lamour (IJL), Ecole des Mines de Nancy, Parc de Saurupt, CS 14234, 54 042 Nancy, France. Jacques Callot (c. 1592 – 1635) was a draftsman that was working in Nancy and important figure in the development of the old master print (engraving, etching…)Stanislas place in Nancy
    •  Introduction what is patterning and why surface patterning? Strategies for creating surface patterns  Photolithography  Advanced serial mask-less processes  Additive parallel processes with masks (templates)  Removal serial and parallel processes : energy beams Moving parallel processes : patterning by nitriding Last experiments done on combining stainless steel patterning by photolithography and nitriding Conclusion
    • Introduction: what is surface patterning? Surface patterning, also known as surface texturation or surface structuration is a part of surface engineering that consists in the production of a "patterned" surface with some regular array of surface height features on the size scale of several micrometers to some nanometres Integrated 3D gold nanoboxes Austenitic stainless steel patterning by plasma assisted diffusion treatments Deposition of SiOx by atmospheric pressure CVD with localized remote plasmaNbOx nano-pilar with a mushroom-like shape prepared by using ultra-thin alumina mask t=3s t =10 s
    • Introduction: Why creating surface pattern? Bio-inspired structured surfaces Shark skin effect Lotus effect Gecko (Tarentola mauritanica) Corse, FranceS.J. Abbott, P.H. Gaskell, Proc. IMechE, Part C, J. Mechanical Engineering Science, 221 (2007) 1181
    • Introduction: Why creating surface pattern? Wp Wh h s h : height of the patterned layer, s : period of the patterned layer Wp: length of the protrusion, Wh: length of the cavity Aspect ratio h/s µm 4 3.8Bio-inspired structured surfaces: 3.6 Drag reduction in air and water : Shark skin effect… 3.4Lotus effect, Gecko, Cicada wings… 3.2 3 aeronautics, microfluidics…Self-cleaning and antireflective surfaces 2.8 2.6 2.4 2.2 2 1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 Nanodots Tribology (Lubrication…) Magnetic data storage Piston ring in automotive…T. Czerwiec, “Patterning of metals for surface engineering: from top-down towards self assembly”, conferencepresented at the 61th workshop of the international union for vacuum science, technique and applications (IUVTA)
    • Application of patterned surfaces to drag reduction NASA Langley Research Centre (USA) Shear stress with (t) and without (t0) riblets Drag reduction S+ dimensionless riblet spacing ONERA/CERT (France) Use of riblets Wind tunnel experiments Fly tests with 3M (Mach riblets on a Drag reduction in number 1:11 scale of an Airbus the range 5 -8% 0.77-0.79) on an A-320 for bladelike ribs Airbus A- with h/s ≥ 0.6 320 100 ≤ h ≤ 200 mm aircraftD.W. Bechert, M. Bruse, W. Hage, R. Meyer, Naturwissenschaften, 87 (2000) 157P.R.Viswanath, Progress in Aerospace Sciences, 38 (2002) 571
    • Application of patterned surfaces to magnetic data storageOverview of granular versus the patterned media for data storage Hard disk drive Co dots h = 20 nm s = 350 nm Superparamagnetic effect limits the size of a bitA.O. Adeyeye, N. Singh, J. Phys. D, 41 (2008) 153001R. Luttge, J. Phys. D, 42 (2009) 123001E.A. Dobisz, Z.Z. Bandic, T.W. Wu, T. Albrecht, Proc. IEEE, 96 (2008) 1836
    • Application of patterned surfaces to tribology (lubrication) Stribeck curve Comparison between flat surfaces and textured surface produced by laser surface texturing Pin-on-disk friction test Elastohydrodynamic (steel ball, load 0.16 to or mixed lubrication 1.6 Pa, speed 0.015 to (moderate wear) 0.75 ms-1)Boundary lubrication Full-film lubrication (sever wear) (negligible wear) m: friction coefficient Higher lubricant film thickness h = 5.5 mm s =200 mm Dimples density h.v/P: viscosity. speed/pressure 12%A. Kovalchenko, O. Ajayia, A. Erdemir, G. Fenske, I. Etsion, Tribology International, 38 (2005) 219.
    • Application of patterned surfaces to tribology (lubrication) Better with dimples with low area coverage (10 to 15%) and h/s < 0.02 to 0.03 for s around 100 mm Application to piston ring in automotive h = 9-10 mm s =100-110 mm Dynamometer tests on a compression engine have shown 4% lower fuel consumption for textured piston rings Patterned surfaces leads to an improvement in load capacity, wear resistance, friction coefficient etc.. They can act as oil reservoirs and entrap wear particles (in either lubricated or dry sliding) They aid in the film formation of lubricant oil They act as micro-reservoir for lubricant in case of starved lubrication conditions. Surface patterning can be combined Application in sliding guideways of machine tools with deposition of lubricant layers Sliding contact elements Magnetic storage disc surfaces (MoS2, DLC…) Mechanical face sealshttp://www.appropedia.org/Laser_surface_texturing#cite_note-nine-8I. Etsion, E. Sher, Tribology International, 42 (2009) 542
    • Strategies for creating surface patterns: top-down, bottom-up, self-assemblyWith or without mask (template) ? Serial or parallel?
    • Strategies for creating surface patterns  Adding material: the patterned surfaces are created by addition of material to the desired surface, creating small areas of relief.  Removing material: the patterned surfaces are produced by removal of material of the surface, creating small depressions. Metal  Moving material: the change in the surface structure is attributable to elastic or patterning plastic deformation and redistribution of material from some parts of the surface to others.  Self-forming: a disordered system of components, already on the surface or brought to the surface, forms an organized pattern as a consequence of specific, local interactions among the components themselves.K.P. Rajurkar, G. Levy, A. Malshe, M.M. Sundaram, J. McGeough, X. Hu, R. Resnick, A. DeSilva, Annals of theCIRP, 55 (2006) 643Bruzzone A.A.G., Costa H.L., Lonardo P.M., Lucca D.A., CIRP Annals. Manufacturing Technology 57 (2008) 750
    • Elaboration techniques: photolithography as a standard top-down approach Substrate covered by a photosensitive material resist Mask with the pattern to be transferred Mask generation Writing with a rigid stylus (micromachining, STM, AFM… Etched Si with a gold layer as a mask Writing with a beam (photons, electrons, ions) Writing with an electric field, or a magnetic field Gold deposition through a polymeric mask Resolution below 500 nm and around 45S. Roy, J. Phys. D, 40 (2005) R413 to 25 nm for DUV and EUV lithographyM. Geissler, Y. Xia, Adv. Mater., 16 (2004) 1249R. Luttge, J. Phys. D, 42 (2009) 123001
    • Advanced serialmask-less processes
    • Advanced serial mask-less processes Electro-physical and electro-chemical processes Electro-physical process (dielectric liquid) Electro-chemical process (conductive liquid: electrolyte) Micro-electro-discharge machining Chemical reactions with electron transfer across an interface Mn+ + n e- ↔ M0 Electrochemical printing (EcP) Mn+ + n e- → M0 Electrochemical dissolution or machining M0 →Mn+ + n e- Classical ECM use masks for localize etchingS.Roy, J. Phys. D, 40 (2005) R413K.P. Rajurkar, G. Levy, A. Malshe, M.M. Sundaram, J. McGeough, X. Hu, R. Resnick, A. DeSilva, Annals of the CIRP, 55 (2006) 643Chakravarty Reddy Alla Chaitanya, Kenichi Takahata, J. Micromech. Microeng., 18 (2008) 105009
    • Advanced serial mask-less processes Elaboration techniques: other processesElectrochemical micro-patterning with nano-second voltage pulses Other add-on processes  Laser induced chemical vapor deposition (LCVD)  Focused beam (ions or electrons) CVD  Inkjet printing  Dip-pen nanolithography  Electro-hydrodynamic atomization 3M HCl/6M HF electrolyte with a 143 ns pulse Electrochemical nano-patterning by scanning tunneling microscope (STM) Ni sheets patterned by W STM tips 0.2M electrolyte with 2 ns pulsesS.Roy, J. Phys. D, 40 (2005) R413R. Schuster, ChemPhysChem, 8(2007) 34.K.P. Rajurkar, G. Levy, A. Malshe, M.M. Sundaram, J. McGeough, X. Hu, R. Resnick, A. DeSilva, Annals of the CIRP, 55 (2006) 643L. Cagnon, V. Kirchner , M. Kock, R. Schuster1, G. Ertl1, W. T. Gmelin, H. Kück, Z. Phys. Chem., 217 (2003) 299M. Geissler, Y. Xia, Adv. Mater., 16 (2004) 1249
    • Advanced serial mask-less processes (self-assembly?) Serial mask-less processes : localized PACVD Gases Metal tube HV DC  Cu wire 450MHz ~ ~ Capillary ( 100 µm) ~3 mm ‟Tower‟ of hydrocarbon deposited by microjet CVD „Tower‟ of tungsten oxide deposited by wire spraying (10 s, 8 sccm acetylene, 0.25 mm capillary, 8.4 mm away from the substrate, 12 W rf) The peak is 2.4 mm high.Y. Shimizu et al., Surf. Coat. Technol. 200 (2006) 4251A. Holländer and L. Abhinandan, Surf. Coat. Technol. 174-175 (2003) 1175
    • Advanced serial mask-less processes (self-assembly?) Serial mask-less processes : localized PACVD Using self-assembly The formation of these self-organized structures may be explained by the presence of strong electromagnetic EM fields at the processing surface.A. Holländer and L. Abhinandan, Surf. Coat. Technol. 174-175 (2003) 1175D. Mariotti, V. Svrcek, D.G. Kim, Appl. Phys. Lett., 91 (2007) 18311.
    • Advanced serial mask-less processes (self-assembly?) Serial mask-less processes : localized PACVD Atmospheric pressure CVD by localized remote plasma Ar-10%O2 (275 sccm) Plasma Power: ~120 W Hole diameter: 400 µm Ar-0.17% HMDSO (200+30 sccm) HMDSO inner wall plasma of the cavity Ar-10%O2
    • Advanced serial mask-less processes (self-assembly?) Serial mask-less processes : localized PACVD Atmospheric pressure CVD by localized remote plasma « nest-like » structure From hexagonal walls SiOx 200 nm to 6 µm Between 0.5 et 5mm nano-dots pleated film 19
    • Additive parallel processes With masks (templates)
    • Advanced parallel processes with mask (directed self-assembly) Additive processes : nano-patterning using ultra-thin alumina masks (UTAM) Electrochemical method combined with nano- patterning techniques  Highly ordered porous aluminum oxide layers can be formed in optimized acid electrolytes  Pore diameter (10-200 nm) and cell size (25-420 nm) with an hexagonal arrangement  Membranes formed in these nano- porous anodic aluminum oxide can be used as templates Fabrication process of attached UTAMs Fabrication process of connected UTAMsH. Masuda, K. Fukuda, Science, 268 (1995) 1466 and H. Masuda, M. Satoh, Jpn J. Appl. Phys., 35 (1996), L126Yong Lei, Weiping Cai, Gerhard Wilde, Progress in Materials Science, 52 (2007) 465
    • Advanced parallel processes with mask (self-assembly) Additive processes : building blocks Block copolymers Different types of building blocks Colloidal or nanosphere particles Honeycomb and isolated-island Cu Nanolithography for Co patterns. dots array fabrication Cu patterns with 500 nm interval (electroless plating in CuSO4/HF)J.Y. Cheng, C.A. Ross, H. I. Smith, E.L. Thomas, Adv. Mater. 18 (2005) 2505T.W. Haley, Nanotechnology, 14 (2003) R39Hidetaka Asoh, Seiji Sakamoto, Sachiko Ono, J. Colloid Interface Science, 316 (2007) 547
    • Removal serialand parallel processes : energy beams
    • Removal serial mask-less processes Energy beam processes : laser direct imaging Metal drilling process Metal writing process Multi-scaled zirconia Piston ring (steel) texturation by direct laser imaging (ZrO2) coating on a Ti-6Al-4V alloy substrate. ZrO2 powder was mixed with a water-based organic solvent and was sprayed onto Ti- 6Al-4V substrates and fused with a pulsed Nd:YAG laser operated at 10 kHz and at a constant power of 25 W.S. Roy, J. Phys. D, 40 (2005) R413P. G. Engleman, A. Kurella, A. Samant, C. A. Blue, N. B. Dahotre, JOM (2005) 46I. Etsion, E. Sher, Tribology International, 42 (2009) 542
    • Removal serial mask-less processes Energy beam processes : laser shock peening Creation of micro dent (dimples) arrays on a titanium alloy by laser shock peening 0,5 mm Y.B. Guo, R. Caslaru, Fabrication and characterization of micro dent arrays produced by laser shock peening on titanium Ti–6Al–4V surfaces , Journal of Materials Processing Technology 211 (2011) 729–736
    • Removal and moving serial mask-less processes Energy beam processes : laser sub-surface patterning (3D) Nd:YAG laser pulse, peak power density of 1 MW/cm2 Stainless steel substrate Potential applications : security marking, micro- devices based on porous materials : micro-heater, micro-insulator and micro-sensor.Z. L. Li, T. Liu, C. C. Khin, A. C. Tan, L. E. Khoong, H. Y. Zheng, W. Zhou, Direct patterning in sub-surface of stainless steel using laserpulses, OPTICS EXPRESS 18 (2010) 15990.
    • Removal and moving parallel mask-less processes Energy beam processes : laser interference metallurgy  Laser interferences are obtained from the interaction of two or three laser beams  The interference pattern covers the size corresponding to the beam diameter  The obtained textured surfaces are the negative of the interference pattern (molten of metal at the interference maxima)  No mask and no etchingM. D‟Alessandria, A. Lassagni, F. Mücklich, Applied Surface Science, 255 (2008) 3210M. Duarte, A. Lassagni, R. Giovanelli, J.Narciso, E. Louis, F. Mücklich,, Advanced Engineering Materials, 10 (2008) 554
    • Removal and moving parallel mask-less processes Energy beam processes : laser interference metallurgy Line-like periodic pattern Two laser beams Cross-like structures, two laser beams → line-like structures Dot-like periodic pattern Sample rotation 90°, two laser beams → cross-like structures Three laser beamsM. D‟Alessandria, A. Lassagni, F. Mücklich, Applied Surface Science, 255 (2008) 3210M. Duarte, A. Lassagni, R. Giovanelli, J.Narciso, E. Louis, F. Mücklich,, Advanced Engineering Materials, 10 (2008) 554
    • Removal parallel mask-less processes Energy beam processes : Ion beam µm Rapid neutrals 1.5  1.4 1.3 Ar+ 1.2 or 2  1.1 1 0.9 High ion energy (1 keV) N 0.8 0.7 0.6  Sputtering 0.5 0.4 Negative transfer to the 0.3 0.2 substrate 0.1 0 « Patterning of magnetic structures on austenitic stainless steel by local ion beam nitriding » SEM MFM Magneto-optic KerrE. Menendez, A. Martinavicius, M.O. Liedke, G. Abrasonis, J. Fassbender, J. effect (MOKE)Sommerlatte, K. Nielsch, S. Surinach, M.D. Baro, J. Nogue´s, J. Sort, Acta magnetometryMaterialia 56 (2008) 4570.
    • Moving parallel processes : Patterning by nitriding Toward stress patterning engineering
    • Moving parallel processes with mask Surface Patterning by plasma assisted nitriding at low ion energy Dilatational or compositional strain (ec) Nitrided layer Nitrided layer (with nitrogen) virtually removed from the substrate (without stress and nitrogen) Fcc lattice Substrate Substrate Nitrogen introduction Nitrided layer (with nitrogen) virtually removed from the substrate Dx s e Internal stress necessary Substrate action on the layer to return film to substrate dimension Stress and anisotropic strain Dilatational or Elastic strain (ee) Internal stress (s) compositional strain (ec) Without mask With a mask N N Initial interface Elastic and/or plastic deformation induced by nitrogen incorporationT. Czerwiec, G. Marcos, T. Thiriet, Y. Guo, T. Belmonte, to be published in IOP Conference Series: Materials Science and Engineering
    • Moving parallel processes with mask Surface Patterning by plasma assisted nitriding at low ion energy µm 0.75 0.7 0.65 0.6 0.55 0.5 0.45 0.4 0.35 0.3 0.25 0.2 0.15 0.1 50 mm 0.05 0 50 mm
    • Principle of surface patterning by plasma assisted nitriding Remote plasma assisted nitriding microwave power supplyGauge Gas Copper TEM Grids inlet N N N N N N Antenna N N N 360 mm Grid: mesh side Substrate of 200 * 200 µm2 holder 450 mm Initial interface (AISI 316L) Micropatterning! With a mask Primary and turbomolecular pump Elastic and or plastic deformation induced by nitrogen incorporation
    • Exemple of surface patterning by plasma assisted nitriding  Plasma: 60% N2 + 40% H2  Pressure: 5.75 Pa  Substrate temperature: ~ 400 C  Process duration: 1h 10 µm Cross section of a step Extraction of profiles : Surface profilometry µm µm 1 0.8 0.6 0.6 0.4 20000 0.55 0.2 0 0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 µm 0.5 12000 Grids 0.45 Profondeur maximale Valeurs moyennes sur 11 créneaux. High step mean : ~240 nm 0.333 µm Profondeur moyenne 0.23 µm No grids 16000 Largeur 49 µm 0.4Intensity [A.U.] µm 10000 0.35 1 0.8 12000 0.3 0.6 8000 0.25 0.4 0.2 0.2 0 8000 0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 µm 6000 0.15 1 2 3 4 5 6 7 Profondeur maximale 0.314 µm 0.257 µm 0.274 µm 0.209 µm 0.303 µm 0.266 µm 0.361 µm 0.1 Profondeur moyenne Largeur High step mean : ~275 nm 0.266 µm 250 µm 0.255 µm 27.8 µm 0.273 µm 27.8 µm 0.207 µm 27.8 µm 0.289 µm 27.8 µm 0.259 µm 27.8 µm 0.313 µm 250 µm 4000 4000 0.05 46 48 50 52 54 56 58 60 62 64 0 2 X-ray diffraction patterns 2 µm 30 µm Cross section of one dot
    • Silicon oxide layer patterned: procedure (coll LPN) UV photolithography AISI 316L PECVD Spin coatingPolished like-mirror N2O/SiH4 AZ5214 photoresist CCP RIE CCP RIE SF6 /CHF3 O2
    • Patterned mask: features and characteristics AFM picture (height mode) µm 1.5 1.4 1.3 1.2 1.1 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 µm 1 SEM picture 0.8 500 nmCylindrical dots with diameters from 3 to 15 µm 0.6 0.4 0.2 0 0 2.5 5 7.5 10 12.5 15 17.5 20 22.5 25 27.5 30 32.5 35 37.5 40 42.5 45 47.5 µm
    • Patterned mask and expanded austenite Dots after nitriding in MDECR: 4 h. at 400 °C (80% N2 – 20 H2), bias 0 V µm Longueur = 50.0 µm Pt = 0.983 µm Echelle = 1.00 µm µm 0 10 20 30 40 µm 1 0 1.4 0.8 500 nm 5 1.3 500 nm 0.6 10 1.2 1.1 0.4 15 1 0.2 20 0.9 0 0.8 0 2.5 5 7.5 10 12.5 15 17.5 20 22.5 25 27.5 30 32.5 35 37.5 40 42.5 45 47.5 µm 25 0.7 µm 30 0.6 0.5 1.4 35 0.4 1.3 40 0.3 1.2 45 0.2 1.1 0.1 1 0 µm 0.9 0.8 0.7µm Longueur = 50.0 µm Pt = 0.843 µm Echelle = 1.00 µm 0.6 1 0.50.8 500 nm 550 nm 0.40.6 0.30.4 0.2 0.10.2 AFM picture 0 0 0 2.5 5 7.5 10 12.5 15 17.5 20 22.5 25 27.5 30 32.5 35 37.5 40 42.5 45 47.5 µm In such conditions, the nitrided layer is 5.6 to 6 µm thick and we are waiting for a 500 nm to 600 nm expansion (same height for SiO2 dots What happens? and substrate)
    • Patterned mask and expanded austenite Dots after nitriding in MDECR: 4 h. at 400 °C (80% N2 – 20 H2), bias 0 VDot with a diameter of 7 µm Dot with a diameter of 15 µmNo strongly distortion A toroidal-shell shape!
    • Patterned mask and expanded austenite Dots after nitriding in MDECR: 4 h. at 400 °C (80% N2 – 20 H2), bias 0 V Dots 1000 Nitrided parts Nitrided parts 900 800 700 600 500 400 300 200 nm to 200 750 nm 100 0 -100 500 nm -200 300 nm -300 to -400 900 nm -500 0 10 20 30 40 50 60 70 80 90 100 110 Expansion of the nitrided layer (as expected) Vertical movement of the SiO2 dots (totally for the smaller ones; at edges for the bigger) What is the role of expanded austenite ?
    • Patterned mask and expanded austeniteSEM cross-sections after 2 nitriding processes in MDECR: 4 h. at 400 °C (80% N2 – 20 H2), bias 0 V Dot Expanded austenite Austenite  For the small dots: nitrogen completely diffuses under the mask  For the big dots: only a diffusion under mask edges
    • Progressive mask distortion Dots with 800 nm of thick. Same shapes.
    • Progressive mask distortion Different nitriding steps at 400 °C (80% N2 – 20 H2) 1400 4h 1200 6h 1000 8h 10h 800 600 400nm 200 0 -200 -400 -600 -800 4 4 4 4 5 0,0 2,0x10 4,0x10 6,0x10 8,0x10 1,0x10 nm
    • After 10h nitriding 4h 6h 10h
    • CONCLUSIONSurface patterning was introducedSome applications of surface patterning (drag reduction, lubrication, self-cleaning andmagnetic data storage) were presented to show the importance of shape and aspect ratioin surface patterningBased on an tentative classification of strategies for surface patterning, differentelaboration techniques were presented (photolithography, advanced serial mask-lessprocesses, advanced parallel processes with masks, advanced parallel mask-lessprocessesFinally, a strain driven patterning method developed by us was presented: austeniticstainless steel patterning by plasma assisted diffusion treatments:
    • ACKNOWLEDGMENTS IJL “ESPRIT” team