Continuous Production of Nanoparticles using Laser Radiation

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1 Continuous Production of Nanoparticles using Laser Radiation Niko Bärsch Stephan Barcikowski Boris Chichkov NanoDay, October 6th, 2005

2 Laser Zentrum Hannover e.v. Founded in 1986 Staff: approx. 215 people Turnover: 10.9 Mio. (2003) Building built in 1991, annex in 1997 Area: 5700 m², working area: 8900 m² Machine floor: 1400 m², 28 laboratories Board of Directors: Dr.-Ing. A. Ostendorf (CEO) Prof. W. Ertmer (Quantum Optics) Prof. H. Haferkamp (Material Sciences) Prof. H. K. Tönshoff (Production Techn.) Prof. H. Welling (Laser Physics)

3 Industrial Nanotechnology World Market (2001) Ref.: DG-Bank. In: BASF Future Business GmbH 2004

4 World Market of "New" Nanoparticles Ref.: DG-Bank. In: BASF Future Business GmbH 2004

5 Polymer Particle Generation using CO 2 Lasers

6 Metal and Alloy Particle Generation using CO 2 Lasers

7 Continuous Generation of Nanoparticles by UV Laser Cracking of Metal Microspheres

8 LZH Continuous Generation of Nanoparticles by UV Laser Cracking of Metal Microspheres Laser-generated Nanoparticles Raw material: commercial Fe micropowder Excimer Laser (257 nm) "Breaking" 150 µm 500 nm

9 Generation of Titanium Nanoparticle Coatings (Nanofoams) Primary Particle Diameter: nm

10 Influence of Laser Pulse Duration on Laser-Material Interaction: Ablation with Nanosecond Laser Pulses

11 Influence of Laser Pulse Duration on Laser-Material Interaction: Ablation with Femtosecond Laser Pulses

Continuous Generation of Nanoparticles in Gases by Ultrashort-Pulsed Laser Ablation from Solid Targets Experimental Setup CCD Electrical Low-Pressure Impactor (ELPI) P Beam Strahlteiler Splitter

12 Continuous Generation of Nanoparticles in Gases by Ultrashort-Pulsed Laser Ablation from Solid Targets Experimental Setup CCD Electrical Low-Pressure Impactor (ELPI) P Beam Strahlteiler Splitter Linse Lens Laser Sample V ELPI Chamber Kammer Sample Holder P particle analysis by low pressure impaction particle size: µm number of platforms: 12 (el.) / 13 (total) platform pressure: 100 mbar

Continuous Generation of Nanoparticles in Gases by Ultrashort-Pulsed Laser Ablation from Solid Targets Experimental Setup Process Chamber CCD Window Sample Exit Beam Strahlteiler Splitter P Linse

13 Continuous Generation of Nanoparticles in Gases by Ultrashort-Pulsed Laser Ablation from Solid Targets Experimental Setup Process Chamber CCD Window Sample Exit Beam Strahlteiler Splitter P Linse Lens Laser Sample V ELPI Chamber Kammer Sample Holder P Inlet Sample Holder continuous ablation of any solid target material (e.g. titanium, silver, alloys, ) adjustable process no precursors (chemichal raw material) necessary

14 Continuous Generation of Nanoparticles in Gases by Ultrashort-Pulsed Laser Ablation from Solid Targets 25,00 Size distribution Magnesium- 50mW for Mg (50 mw) Magnesium 50 mw 80,00 30,00 Size distribution Titanium- for 50mW Ti (50 mw) Titanium 50 mw 80,00 particle number distribution [%] particle number distribution [%] 20,00 15,00 10,00 5,00 70,00 60,00 50,00 40,00 30,00 20,00 10,00 mass distribution [%] mass distribution [%] particle number distribution [%] particle number distribution [%] 25,00 20,00 15,00 10,00 5,00 70,00 60,00 50,00 40,00 30,00 20,00 10,00 mass [%] mass distribution [%] 0, aerodynamic particle diameter [nm] aerodynamic particle diameter [µm] aerodynamic particle diameter [µm] 0,00 0, aerodynamic particle diameter particle [nm] diameter [µm] aerodynamic particle diameter [µm] 0,00 monomodal particle size distribution majority of particles on the nano-scale particles adjustable by process parameters

Pulses Green: Red: Laser Beam Wavelength (532 nm) Plasmon Resonance

15 Generation of Gold Nanoparticle Colloids using ps Laser Pulses Video: Generation of Gold Nanoparticles using Ultrashort (Picosecond) Laser Pulses Green: Red: Laser Beam Wavelength (532 nm) Plasmon Resonance of Gold Nanoparticles Time: 0 s Time: 36 s SEM Time: 108 s Time: 144 s

16 Geometry of Gold Nanoparticles from Femtosecond Laser Ablation Cumulative Frequency [%] Particle Number Cumulative Frequency Particle Number Distribution [%] nm Geometric (TEM) Diameter [nm]

17 VIS Plasmon Resonance of fs-laser-generated Gold Nanoparticles

18 Absorption from Gold Nanoparticles at the Example of the Notre Dame in Paris glass with different amounts of silver and gold nanoparticles

Absorption from Gold Nanoparticles at the Example of the Roman Lycurgus Cup (British Museum) glass with small amounts of silver (300 ppm) and gold (40 ppm) with a

19 Absorption from Gold Nanoparticles at the Example of the Roman Lycurgus Cup (British Museum) glass with small amounts of silver (300 ppm) and gold (40 ppm) with a diameter of about 70 nm green in reflected light (daylight), red by transmitted light perhaps manufactured by accident using an ingredient containing silver and gold

Modification of the Optical Characteristics Ag/Au Co-Colloid Ag Ag/Au Au 90 80 70 100% Ag: 200mW, 200µJ, 33% Ag, 66% Au: 100mW, 100µJ 11% Ag, 89% Au: 100mW, 100µJ Ag (Kik et al.

20 Modification of the Optical Characteristics Ag/Au Co-Colloid Ag Ag/Au Au % Ag: 200mW, 200µJ, 33% Ag, 66% Au: 100mW, 100µJ 11% Ag, 89% Au: 100mW, 100µJ Ag (Kik et al.): λ Res =410nm, τ relax ~10 fs Absorption / % Wavelength: 780 nm Pulse Length: 150 fs Repetition Rate: 1 khz Processing Time: 480 s TEM: A. Feldhoff / Caro, PCI, Uni Hannover λ / nm

21 LZH SEM Analysis of Femtosecond-Laser Generated Silver Nanoparticles HR-SEM: J. Becker, Institut für Festkörperphysik, Uni Hannover

independence) of diffusion as the key to quality control:

22 Analysis of Silver Nanoparticles in Water by Laser Light Diffusion Measurement Video Size dependence (and material independence) of diffusion as the key to quality control: Particle Trajectories D t = K B T / 6πηr h (Analysis provided by NanoSight)

23 Examples of fs-laser-generated Nanoparticles

Femtosecond-Laser-Generated Stoichiometric

EDX analysis Fe : Ni ~ 1:1 Permalloy: Trademark

24 Femtosecond-Laser-Generated Stoichiometric Nanoparticles Alloy: FeNi (47.5 / 47.5) + Si + Mn Generation of Nanoparticles using Direct Femtosecond Laser Ablation of Permenorm TM EDX analysis Fe : Ni ~ 1:1 Permalloy: Trademark of Vakuumschmelze GmbH, Germany Analysis provided by PZH, Uni Hannover

25 Summary (I) (Nanosecond) UV Laser Cracking of Microspheres Generation of Layers/Coatings (e.g. Titanium-Nanofoams) Production Rate: mg/h g/h Picosecond Laser Ablation Ablation of Bulk Material in Liquids (Gold in Water) Production Rate: mg/h Femtosecond Laser Ablation (Stoichiometric) Ablation of Bulk Material in Liquids (Metals, Metal Oxides, Alloys) Production Rate: µg/h - mg/h

26 Summary (II) Characteristics of Ultrashort-Pulsed-Laser Nanoparticle Generation No Chemical Precursors Stoichiometric Conversion (e.g. of Alloys) into Nanoparticles Continuous Process Online Process Control Possible (e.g. using ELPI, Plasmon Resonance) Assignments Control of the Size Distribution Comparably Low Production Rates Ablation in Polyols, Direct Coating Positive Economic Balance only for High Added Value Materials Process Qualification for Direct Coating and Bio-conjugation

Nanophysics: Main trends

Nano-opto-electronics Nanophysics: Main trends Nanomechanics Main issues Light interaction with small structures Molecules Nanoparticles (semiconductor and metallic) Microparticles Photonic crystals Nanoplasmonics