Surface Functionalization by Atomic Layer Deposition

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1 Surface Functionalization by Atomic Layer Deposition Christophe Detavernier SIM User Forum - Gent 27/10/2015 CoCooN Conformal Coating of Nanomaterials

2 Atomic layer deposition (ALD) Gas-phase thin film deposition technique Cyclic process of self-limiting surface reactions layer-by-layer growth TMA pulse Self-saturated chemisorption Example : ALD growth of Al 2 O 3 from trimethyl aluminum (TMA) and H 2 O One (sub)monolayer of Al 2 O 3 New OH groups at the surface Water pulse 2

3 Thickness (Angstrom) Advantages and limitations of ALD Layer-by-layer deposition Advantages of ALD Ultimate control of layer thickness Excellent conformality Excellent control of stoichiometry Highly uniform Easily upscalable Growth rate per cycle from linear fit 0.85 Angstrom/cycle Cycle number Limitations of ALD Slow limited to nanocoatings and surface engineering 3

4 Materials that can be deposited by ALD Many different materials demonstrated Puurunen et al., J. Appl. Phys. 97, (2005). 4

5 Advantages and limitations of ALD Layer-by-layer deposition Advantages of ALD Ultimate control of layer thickness Excellent conformality Excellent control of stoichiometry Highly uniform Easily upscalable Limitations of ALD Slow limited to nanocoatings and surface engineering ALD is ideal tool for 3D surface engineering Controlling surface properties: adhesion, friction, hydrophobicity Surface functionalization: catalysis Surface passivation: diffusion barriers, encapsulation, anticorrosion 5

6 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 6

7 Functional nanocoatings in micro-electronics 7

8 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 8

9 ALD nanocoatings for encapsulation: Protecting silver objects from tarnishing Problem: silver objects require cleaning after some time ALD solution: 10nm Al 2 O 3 sapphire-like coating Accelerated tarnishing test: uncoated ALD coated 9

10 ALD can be scaled to large batches 10

11 ALD nanocoatings for encapsulation: Protecting CaS:Eu phosphor powders from moisture Avci et al., J. Electrochem. Soc. 156(11) J333 (2009). 11

12 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 12

13 ALD for surface engineering: Making a Kleenex tissue hydrophobic Original tissue ALD coated tissue (200 cycles Al 2 O 3 ) Thermal ALD, TMA + H 2 O, 50 C 13

14 ALD for surface engineering: Making Teflon hydrophilic. + High thermal stability (melting at C) + High chemical resistance + Low coefficient of friction + Low dielectric loss (RF applications) - Poor adhesion, not glueable - Lack of reactivity makes it challenging to functionalize the PTFE surface Native Teflon - hydrophobic ALD coated Teflon - hydrophilic Patent application (WO A1) A. K. Roy et al., Chem. Commun. 2015, 51,

15 Patent application (WO A1) A. K. Roy et al., Chem. Commun. 2015, 51, ALD for surface engineering: Making Teflon gluable. Average Load (N) fold improvement of adhesion after PE-ALD 10 Scotch tape on Aluminum Native PTFE Thermal ALD Plasma enhanced ALD 5 20mm wide strips Peeling speed 5 mm/s Peeling angle Number of Cycles

16 Patent application (WO A1) A. K. Roy et al., Chem. Commun. 2015, 51, ALD for surface engineering: Making Teflon gluable. Aluminum plate superglue PTFE sheet Uncoated PTFE peels off Native Teflon Poor adhesion PE-ALD coated Teflon glueable!!

17 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 17

18 ALD coating of nanoporous materials for catalysis ALD coating throughout the interior surface of a nanoporous material

19 Photocatalysis ALD of amorphous TiO 2 inside mesoporous silica particles Calcination leads to uniformly distributed anatase TiO 2 nanoparticles S.P. Sree, J. Dendooven, K. Masschaele, H.M. Hamed, S. Deng, C-ALD Meeting 2014, Shanghai 19 S. Bals, C. Detavernier, J.A. Martens, Nanoscale, 2013,5,

20 Photocatalysis 1.0 Methylene blue C(t)/C Porous film - 0 ALD cycles Porous film - 50 ALD cycles Glass ALD cycles irradiation time (h) Excellent dispersion of anatase particles in accessible mesopores Excellent photocatalytic activity Method can be extended to other metal oxides Potentially useful concept for lab-on-a-chip applications S.P. Sree, J. Dendooven, K. Masschaele, H.M. Hamed, S. Deng, C-ALD Meeting 2014, Shanghai 20 S. Bals, C. Detavernier, J.A. Martens, Nanoscale, 2013,5,

21 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 21

22 Multilayer ALD coating of a carbon nanotube TiO 2 /V 2 O 5 /TiO 2 multilayer coating of a carbon nanotube 22

23 Platinum ALD coating of carbon nanotubes Shaoren Deng, et al., Nanoscale, 2014, 6,

24 Fabrication of Platinum nanowires After calcination : Pt nanoparticles transformed into interconnected nanowires. As deposited Calcined Shaoren Deng, et al., Nanoscale, 2014, 6,

25 Applications of ALD Functional nanocoatings in micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects Powder coating 25

26 ALD for coating powders Particles are 3D objects conformal coating by ALD 5 nm Easy concept: Put a cup of powder in a regular flow-type or pump-type ALD reactor. Problem: Precursors and reactants cannot diffuse easily down to the particle bed! Uncoated particle Coated particle Diffusion time of TMA at 10 mbar pressure in a cubically stacked bed of spherical particles with 100 nm diameter. C-ALD Meeting 2014, Shanghai 26 D. Longrie et al., J. Vac. Sci. Technol. A, 32(1), Jan/Feb 2014.

27 Rotary reactor for thermal and PE-ALD on powders Rotating dielectric tube Turbomolecular pump Furnace Plasma coil (ICP) Precursors and reactants Connection for MS / OES Advantages of PE-ALD: Lower processing temperatures Higher quality coatings Cheaper precursor chemistry available Demonstrated oxide/nitride coatings on oxide/metal particles. D. Longrie et al., J. Vac. Sci. Technol. A, 32(1), Jan/Feb

28 ALD on powders Geldart diagram D. Longrie et al., Surface and Coatings Technology, 213 (2012)

29 FUNC FUNC: Tools for dry nanofunctionalization of particles and fibrous materials 29

30 Summary Atomic layer deposition offers Ultimate thickness control Ultimate conformality Wide range of applications Nanocoatings for micro-electronics Encapsulation Surface engineering hydrophobic/hydrophilic Surface engineering adhesion Coating nanoporous materials for catalysis Coating nano-objects ALD is being explored for powder coating within SIM-FUNC 30

31 ACKNOWLEDGEMENTS 31

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