Nanomaterials for bottom-up manufacturing Jurriaan Huskens
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1 Nanomaterials for bottom-up manufacturing Jurriaan Huskens University of Twente, MESA + Institute for Nanotechnology Molecular Nanofabrication group Enschede, The Netherlands
2 General philosophy Assembly: fundamental applied Patterning: flat stamps fundamental NIL patterning 3D nanostructures applied patterned protein constructions printboards, multivalency, supramolecular nanolithography
3 Molecular printboards CD monolayers on gold: infinite 2D receptor lattices: HO OH O O OH 7 β-cyclodextrin (CD) CA: polarity: θ adv = 55 o EIS: thickness: 2-3 nm XPS: bound sulfur: 65 % SIMS: molecular peaks: (M+Au) + AFM: molecular order: 2.1 nm M. W. J. Beulen, J. Bügler, M. R. de Jong, B. Lammerink, J. Huskens, H. Schönherr, G. J. Vancso, B. A. Boukamp, H. Wieder, A. Offenhäuser, W. Knoll, F. C. J. M. van Veggel, D. N. Reinhoudt, Chem. Eur. J. 2000, 6, 1176
4 Molecular printboards Small guests at a CD monolayer: Δα (º) [guest] (μm) K Δα sat K ΔH TΔS (M -1 ) ( ) (M -1 ) (kcal mol -1 ) (kcal mol -1 ) Fe OH N H N H O O M. R. de Jong, J. Huskens, D. N. Reinhoudt, Chem. Eur. J. 2001, 7, 4164
5 General introduction to multivalency Multivalency at interfaces: Examples in Nature: cell membrane interactions with bacteria and viruses: M. Mammen, S.-K. Choi, G. M. Whitesides, Angew. Chem. Int. Ed. 1998, 37, 2754
6 μcp on SAMs Patterning with multiple multivalent molecules: Confocal microscopy images Em > 600 nm 500 < Em < 530 nm Simultaneous 60 μm S. Onclin, A. Mulder, J. Huskens, B. J. Ravoo, D. N. Reinhoudt, Langmuir 2004, 20, 5460 A. Mulder, S. Onclin, M. Péter, J. P. Hoogenboom, H. Beijleveld, J. ter Maat, M. F. García- Parajó, B. J. Ravoo, J. Huskens, N. F. van Hulst, D. N. Reinhoudt, Small 2005, 1, 242
7 Supramolecular materials Supramolecular layer-by-layer assembly scheme using CD-Au colloids and adamantyl-functionalized dendrimers: + G5 dendrimer O. Crespo-Biel, B. Dordi, D. N. Reinhoudt, J. Huskens, J. Am. Chem. Soc. 2005, 127, 7594 Layer-by-layer assembly: G. Decher, Science 1997, 277, 1232
8 Supramolecular materials Supramolecular building blocks for LBL assembly: OH Adamantyl dendrimers: O O HO OH 7 β-cyclodextrin Molecular printboards: J. J. Michels, M. W. P. L. Baars, E. W. Meijer, J. Huskens, D. N. Reinhoudt, J. Chem. Soc., Perkin Trans. 2, 2000, J. Huskens, M. A. Deij, D. N. Reinhoudt, Angew. Chem. Int. Ed. 2002, 41, 4467; T. Auletta, B. Dordi, A. Mulder, A. Sartori, S. Onclin, C. M. Bruinink, C. A. Nijhuis, H. Beijleveld, M. Péter, H. Schönherr, G. J. Vancso, A. Casnati, R. Ungaro, B. J. Ravoo, J. Huskens, D. N. Reinhoudt, Angew. Chem. Int. Ed. 2004, 43, 369
9 Supramolecular materials Supramolecular building blocks for LBL assembly: Cyclodextrin gold nanoparticles: SH HO O OH O 7 + HAuCl 4 NaBH 4 DMSO CH 3 CN TEM: diameter 2.8 ± 0.6 nm J. Liu, W. Ong, E. Román, M. J. Lynn, A. E. Kaifer, Langmuir 2000, 16, 3000 Supramolecular multivalent aggregation: Au O. Crespo-Biel, A. Juković, M. Karlsson, D. N. Reinhoudt, J. Huskens, Isr. J. Chem. 2005, 45, 353
10 Supramolecular materials Layer-by-layer assembly using CD-Au colloids and Ad dendrimers: SPR spectroscopy: Norm.Intensity at Detector time (min) Solutions: 6.5 μm CD-Au (H 2 O) 0.01 mm Ad-G5 (1 mm CD ph 2) Rinse 1 mm CD ph 2 Rinse H 2 O O. Crespo-Biel, B. Dordi, D. N. Reinhoudt, J. Huskens, J. Am. Chem. Soc. 2005, 127, 7594
11 Supramolecular materials A Layer-by-layer assembly using CD-Au colloids and Ad dendrimers: UV/Vis at glass substrates: Quantitative interpretation possible: 1 monolayer of particles per bilayer bilayers A at 534 nm λ (nm) O. Crespo-Biel, B. Dordi, D. N. Reinhoudt, J. Huskens, J. Am. Chem. Soc. 2005, 127, # bilayers
12 3D Supramolecular materials Towards patterned LBL assemblies: 3D Nanofabrication: x,y: top-down patterning z: LBL assembly Patterned SAMs: (μcp, NIL) CD silicon inert SAM silicon Patterned gold: (μcp+etching, NIL+metal lift-off, sieve evaporation) CD silicon inert SAM Structures on patterned stamp: (μcp) Patterned mask: (NIL) polymer template CD silicon
13 3D Supramolecular materials Alternative: LBL on PDMS stamp followed by assembly transfer by μcp: PDMS UV/O 3 silicon CDs gold LBL assembly silicon O. Crespo-Biel, B. Dordi, P. Maury, M. Péter, D. N. Reinhoudt, J. Huskens, Chem. Mater. 2006, 18, 2545 LBL in combination with μcp: J. Park, P. T. Hammond, Adv. Mater. 2004, 16, 520
14 3D Supramolecular materials Patterned LBL assemblies by μcp: 20 silicon AFM height image (80 x 80 μm 2 ) 2 bilayers: 7 nm height (nm) # bilayers Assemblies are stable against rinsing with competitive CD solutions AFM height image (60 x 60 μm 2 ) 4 bilayers: 14 nm O. Crespo-Biel, P. Maury, M. Péter, B. Dordi, D. N. Reinhoudt, J. Huskens, Chem. Mater. 2006, 18, 2545
15 Directed nanoparticle assembly on NIL templates Nanofabrication scheme including NIL and directed nanoparticle deposition: T>T g topographical template chemical template T T g chemical template topographical template P. Maury, M. Péter, V. Mahalingam, D. N. Reinhoudt, J. Huskens, Adv. Funct. Mater. 2005, 15, 451
16 Directed nanoparticle assembly on NIL templates Improved particle deposition process: controlled wetting and capillary forces: physical principle vertical NP deposition tool
17 Directed nanoparticle assembly on NIL templates Particle adsorption in PMMA templates using vertical colloidal deposition: 10 μm 1 μm 5 μm lines 1 μm holes 600 nm lines 500 nm P. Maury, M. Escalante, M. Péter, D. N. Reinhoudt, J. Huskens, Adv. Mater. 2005, 17, μm 1 μm 1 μm 500 nm lines
18 Directed nanoparticle assembly on NIL templates Particle adsorption on NIL-patterned SAMs using vertical colloidal deposition: 5 μm lines 1 μm 200 nm lines 5 μm 200 nm P. Maury, M. Escalante, M. Péter, D. N. Reinhoudt, J. Huskens, Adv. Mater. 2005, 17, μm dots 1 μm 1 μm 1 μm dots
19 NIL-patterned molecular printboards NIL-patterned CD monolayers on SiO 2 : templates for multivalent supramolecular adsorption: a) b) c) 1μm 1μm 1μm AFM height: 0.9 nm 0.9 nm 2.8 nm (after polymer removal) P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18,
20 3D Supramolecular materials Integration with layer-by-layer (LBL) assembly: NPs: 2.8 nm CD Au NPs: 60 nm CD SiO 2 Lift-off Lift-off P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18,
21 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: results: NIL-patterned CD SAMs: AFM height image (8 x 8 μm 2 ) no bilayers: 2 nm (7 process steps) NIL-patterned CD SAMs followed by LBL, then polymer removal: AFM height image (30 x 30 μm 2 ) 2 bilayers: 6 nm AFM height image (30 x 30 μm 2 ) 4 bilayers: 10 nm (15 process steps!)
22 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: results: NIL-patterned CD SAMs followed by LBL: submicron patterns: 15 process steps! AFM height image (4 x 4 μm 2 ) 2 bilayers: 5 nm line width: 700 nm AFM height image (2.8 x 2.8 μm 2 ) 4 bilayers: 10 nm line width: 700 nm J. Huskens, P. Maury, O. Crespo-Biel, M. Péter, D. N. Reinhoudt, Proceed. Instit. Mech. Engin. N: J. Nanoengin. Nanosys. 2006, 220, 157 P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18,
23 Height (nm) 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: results using an e-beam made master: AFM 15 bilayers: 37 process steps!! 500 nm 500 nm 500 nm 50 SEM nm 500 nm 500 nm dot width: 200 nm 100 nm 50 nm P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18, Diameter (nm)
24 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: LBL with 60 nm CD SiO 2 NPs: SEM 1-3 bilayers: height = n x 60 nm 2μm 2μm 3 AFM 2μm 2 1 P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18,
25 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: LBL with 60 nm CD SiO 2 NPs: 2 bilayers on line and grid patterns 1 bilayer on dot patterns 1μm 500 nm AFM SEM 500 nm 100 nm P. Maury, M. Péter, O. Crespo-Biel, X. Y. Ling, D. N. Reinhoudt, J. Huskens, Nanotechnology 2007, 18,
26 3D Supramolecular materials NIL-patterned polymer masks for directed LBL: LBL with 3 nm CD Au and 60 nm Fc SiO 2 NPs: Thickness L6 L5 L4 L3 L2 L nm Distance (micron) m thickness (nm) X. Y. Ling, I. Y. Phang, G. J. Vancso, D. N. Reinhoudt, J. Huskens, Int. J. Mol. Sci. 2008, 9, L1 L2 L3 L4 L5 L6 number of bilayer
27 Nanoparticle-substrate interface chemistry Key question: What is the role of the interface chemistry on the assembly (order, reversibility) of large nanoparticles? Case study: 500 nm polystyrene NPs: physisorption electrostatic host-guest X. Y. Ling, L. Malaquin, D. N. Reinhoudt, H. Wolf, J. Huskens, Langmuir 2007, 23, 9990
28 Nanoparticle-substrate interface chemistry Key question: What is the role of the interface chemistry on the assembly (order, reversibility) of large nanoparticles? Setup: Evaporation Particle convective flow Glass slide Movement of substrate Temperature controller Tc ( A ) Assembly Zone ( B) Solution Zone X. Y. Ling, L. Malaquin, D. N. Reinhoudt, H. Wolf, J. Huskens, Langmuir 2007, 23, 9990
29 Nanoparticle-substrate interface chemistry Physisorption: PS-COOH NPs on clean SiO 2 : Assembly zone Solution zone
30 Nanoparticle-substrate interface chemistry Host-guest interaction: PS-CD NPs on CD SAMs with G1 Fc dendrimers: Assembly zone 2 μm Solution zone
31 Nanoparticle-substrate interface chemistry Host-guest interaction: PS-CD NPs on CD SAMs with G1 Fc dendrimers: competition by CD in solution Assembly zone Solution zone
32 Summary Assembly: fundamental applied Patterning: flat stamps fundamental NIL patterning 3D nanostructures applied patterned protein constructions printboards, multivalency, supramolecular nanolithography
33 Acknowledgements Molecular Nanofabrication group: Xing Yi Ling Dr. Olga Crespo-Biel Manon Ludden Dr. Pascale Maury Prof. David Reinhoudt Dr. Maria Peter Dr. Venkataramanan Mahalingam Prof. Bart Jan Ravoo IBM Zurich, Switzerland: Dr. Laurent Malaquin, Dr. Heiko Wolf Transducer Science and Technology, MESA+, University of Twente: Dr. Henri Jansen, Dr. Niels Tas, Prof. Miko Elwenspoek Materials Science and Technology of Polymers, MESA+, University of Twente: Dr. Mark Hempenius, Prof. G. Julius Vancso Financial support:
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