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PHOTONICA 2019, Belgrade, 26-30 August, 2019 M. Trtica 1 , J. Stašić 1 , D. Batani 2 , R. Benocci 3 , V. Narayanan 4 , J. Ciganović 1 1 Institute of Nuclear Sciences “Vinča”, University of Belgrade, Serbia 2 Université Bordeaux, CNRS, CEA, CELIA (Centre Lasers Intenses et Applications), France 3 Università degli Studi di Milano-Bicocca, Italy 4 Indian Institute of Technology Jodhpur, Rajasthan, India e-mail: [email protected] Titanium target irradiation by picosecond laser in air and water surface morphology and synthesis of nanoparticles Titanium target was irraditiated by picosecond lasers with pulse lengths 40 ps and 150 ps in air and water environment. The goal was studying of the induced surface features in both ambiences, as well as synthesis of Ti-based nanoparticles (NPs) in liquid. Morphologies of the target were studied by scanning electron microscope (SEM) and profilometry, while chemical analysis of the surface was done by energy- dispersive spectrometry (EDS). Interaction ps laser-Ti depends on a number of parameters laser parameters, target surface condition, working ambience, etc. Irradiation conditions in this work were as follows: τ=40/150 ps, wavelength 1064 nm, pulse frequency 10 Hz, pulse energy 2-20 mJ, pulse count 3000-9000, irradiation in focusing regime. Generally, induced features differ in air and water surrounding damage is more diffuse in water, with characteristic wavy surface. In both media laser-induced periodic surface structures (LIPSS) are observed on the damage periphery, however they appear at lower pulse count in water. Irradiation of Ti in water led to creation of nanoparticles (NPs) in most cases as established by UV-Vis spectrophotometry, and their size distribution was determined by DLS (dynamic light scattering) analysis. These were, as expected, Ti-oxide NPs as laser ablation in water always leads to formation of oxide particles except in case of noble metals. The size and shape of NPs obtained using laser ablation in liquid (LAL) method depends strongly on the liquid medium used, as well as laser parameters. In our case NPs were spherical, sized from few tens to few hundreds of nanometers, with occurrence of smaller particles in case of 150 ps laser. With further optimization of conditions obtaining of smaller NPs can be expected. REFERENCES [1] C. Langlade, A.B. Vannes, J.M. Krafft, J.R. Martin, Surf. Coat. Technol. 100-101, 383 (1998). [2] V. Amendola, M. Meneghetti, Phys. Chem. Chem. Phys. 15, 3027 (2013). [3] M. Trtica, J. Stasic, D. Batani, R. Benocci, V. Narayanan, J. Ciganovic, Appl. Surf. Sci. 428, 669 (2018). Acknowledgements. The results presented were realized with the financial support of the Ministry of Education, Science and Technological Development of the Republic of Serbia through project no. 172019, and COST-MP1208 Action “Developing the Physics and the Scientific Community for Inertial Confinement Fusion at the Time of NIF ignition”. It should be pointed out that irradiation in water environment enables direct collection of synthesized titanium based nanoparticles (Fig. 3). Nd:YAG laser 4 mm a.f. f. Fig. 3. Exp. setup for synthesis of nanoparticles by laser ablation in liquid. 100 μm Non-irradiated 200 μm 100 μm 100 μm 200 μm 100 μm 100 μm Air 1000 pulses Water 1000 pulses Surface modifications of titanium with 40 ps - laser radiation have shown: (i) Strong dependence on the ambience used; (ii) Air lower damage spot with diffuse character on the periphery. Presence of hydrodynamic and cracking effects. Appearance of LIPSS (Laser Induced Periodic Surface Structures) on the periphery at lower pulse count; Water damage depth is higher. Rough surface, with prominent sponge-like character. LIPSS generation; (iii) Irradiation in both ambiences followed by plasma formation which was more confined in water. Target topography highly impacted by the ambience : damage depth much higher in water (40 μm) than in air (14 μm). Fig. 2. 3D and 2D profilometric analysis. Air atmosphere: E = 17 mJ (Φ 1 ≈ 10.0 J/cm 2 , I 1 ≈ 2.5 × 10 11 W/cm 2 ). Water ambience: E = 17 mJ (Φ 2 ≈ 7.6 J/cm 2 , I 2 ≈ 1.9 × 10 11 W/cm 2 ). Fig. 1. SEM analysis of the Ti-target after 1000 pulses. Air atmosphere: E = 17 mJ (Φ 1 ≈ 10.0 J/cm 2 , I 1 ≈ 2.5 × 10 11 W/cm 2 ). Water ambience: E = 17 mJ (Φ 2 ≈ 7.6 J/cm 2 , I 2 ≈ 1.9 × 10 11 W/cm 2 ). Fig. 4. Size distribution of Ti-based NPs in water and corresponding UV-Vis spectrum - inset. (τ = 40 ps; E = 17 mJ; I≈ 1.9 × 10 11 W/cm 2 ; pulse count 9000) Air (sp. 2*, wt%) Water (sp. 1*, wt%) Non-irrad. region (wt%) C 0.3 0.5 0.4 O / 6.4 0.2 Ti 99.7 93.1 99.4 Total 100 Table 1. Local EDS elemental analysis (after 1000 pulses) in dependence on the used ambience. * Measuring locations (central damage zone) are given in Fig. 1. Fig. 5. Size distribution of Ti-based NPs in water. (τ = 150 ps; E = 17 mJ; I≈ 1.9 × 10 11 W/cm 2 ; pulse count 9000). The action of ps-lasers (τ = 40 ps and τ = 150 ps) induced generation of titanium-based nanoparticles in water more specifically, Ti-oxide NPs spherically shaped. Initial results have shown that longer laser pulses have some advantage (NPs size peak at 100 nm, τ = 150 ps) compared to shorter pulses (NPs size peak 150 nm, τ = 40 ps). Center Center Periphery Periphery 0 mm mm 2.013 2.144 Distance (mm) Height (μm) +5 0 -5 -10 -15 0.0 0.5 1.0 1.5 2.0 mm mm 0 1.631 1.566 Distance (mm) Height (μm) +10 0 -10 -20 -30 -40 -50 0.0 0.5 1.0 1.5 Air Water

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  • PHOTONICA 2019, Belgrade, 26-30 August, 2019

    M. Trtica1, J. Stašić1, D. Batani2, R. Benocci3, V. Narayanan4, J. Ciganović1

    1Institute of Nuclear Sciences “Vinča”, University of Belgrade, Serbia2Université Bordeaux, CNRS, CEA, CELIA (Centre Lasers Intenses et Applications), France

    3Università degli Studi di Milano-Bicocca, Italy4Indian Institute of Technology Jodhpur, Rajasthan, India

    e-mail: [email protected]

    Titanium target irradiation by picosecond laser in air and water – surface morphology and synthesis of nanoparticles

    Titanium target was irraditiated by picosecond lasers with pulse lengths 40 ps and 150 ps in air and water environment. The goal wasstudying of the induced surface features in both ambiences, as well as synthesis of Ti-based nanoparticles (NPs) in liquid. Morphologies ofthe target were studied by scanning electron microscope (SEM) and profilometry, while chemical analysis of the surface was done by energy-dispersive spectrometry (EDS). Interaction ps laser-Ti depends on a number of parameters – laser parameters, target surface condition,working ambience, etc. Irradiation conditions in this work were as follows: τ=40/150 ps, wavelength 1064 nm, pulse frequency 10 Hz, pulseenergy 2-20 mJ, pulse count 3000-9000, irradiation in focusing regime. Generally, induced features differ in air and water surrounding –damage is more diffuse in water, with characteristic wavy surface. In both media laser-induced periodic surface structures (LIPSS) areobserved on the damage periphery, however they appear at lower pulse count in water. Irradiation of Ti in water led to creation ofnanoparticles (NPs) in most cases as established by UV-Vis spectrophotometry, and their size distribution was determined by DLS (dynamiclight scattering) analysis. These were, as expected, Ti-oxide NPs as laser ablation in water always leads to formation of oxide particles exceptin case of noble metals. The size and shape of NPs obtained using laser ablation in liquid (LAL) method depends strongly on the liquidmedium used, as well as laser parameters. In our case NPs were spherical, sized from few tens to few hundreds of nanometers, withoccurrence of smaller particles in case of 150 ps laser. With further optimization of conditions obtaining of smaller NPs can be expected.

    REFERENCES[1] C. Langlade, A.B. Vannes, J.M. Krafft, J.R. Martin, Surf. Coat. Technol. 100-101, 383 (1998).[2] V. Amendola, M. Meneghetti, Phys. Chem. Chem. Phys. 15, 3027 (2013).[3] M. Trtica, J. Stasic, D. Batani, R. Benocci, V. Narayanan, J. Ciganovic, Appl. Surf. Sci. 428, 669 (2018).

    Acknowledgements. The results presented were realized with the financial support of the Ministry of Education, Science and Technological Development of the Republic of Serbia through project no. 172019, and COST-MP1208 Action “Developing the Physics and the Scientific Community for Inertial Confinement Fusion at the Time of NIF ignition”.

    It should be pointed out that irradiation in water environment enablesdirect collection of synthesized titanium based nanoparticles (Fig. 3).

    Nd:YAG laser

    4 mm a.f.

    f.

    Fig. 3. Exp. setup for synthesis of nanoparticles bylaser ablation in liquid.

    100 μm

    Non-irradiated

    200 μm 100 μm 100 μm

    200 μm 100 μm 100 μm

    Air1000 pulses

    Water1000 pulses

    Surface modifications of titanium with 40 ps-laser radiation have shown:(i) Strong dependence on the ambience used;(ii) Air – lower damage spot with diffusecharacter on the periphery. Presence of hydrodynamic and cracking effects. Appearanceof LIPSS (Laser Induced Periodic Surface Structures) on the periphery at lower pulse count;Water – damage depth is higher. Rough surface, with prominent sponge-like character. LIPSS generation;(iii) Irradiation in both ambiences followed by plasma formation which was more confined in water.

    Target topographyhighly impacted bythe ambience :damage depth much higher in water (40 µm) than in air (14 µm).

    Fig. 2. 3D and 2D profilometric analysis.Air atmosphere: E = 17 mJ (Φ1 ≈ 10.0 J/cm

    2, I1 ≈ 2.5 × 1011 W/cm2).

    Water ambience: E = 17 mJ (Φ2 ≈ 7.6 J/cm2, I2 ≈ 1.9 × 10

    11 W/cm2).

    Fig. 1. SEM analysis of the Ti-target after 1000 pulses.Air atmosphere: E = 17 mJ (Φ1 ≈ 10.0 J/cm

    2, I1 ≈ 2.5 × 1011 W/cm2).

    Water ambience: E = 17 mJ (Φ2 ≈ 7.6 J/cm2, I2 ≈ 1.9 × 10

    11 W/cm2).

    Fig. 4. Size distribution of Ti-based NPs in water and corresponding UV-Vis spectrum - inset.(τ = 40 ps; E = 17 mJ; I≈ 1.9 × 1011 W/cm2; pulse count 9000)

    Air (sp. 2*, wt%) Water (sp. 1*, wt%) Non-irrad. region (wt%)C 0.3 0.5 0.4O / 6.4 0.2Ti 99.7 93.1 99.4

    Total 100

    Table 1. Local EDS elemental analysis (after 1000 pulses) in dependence on the used ambience.

    * Measuring locations (central damage zone) are given in Fig. 1.

    Fig. 5. Size distribution of Ti-based NPs in water.(τ = 150 ps; E = 17 mJ; I≈ 1.9 × 1011 W/cm2;pulse count 9000).

    The action of ps-lasers (τ = 40 ps and τ = 150 ps) induced generation of titanium-based nanoparticles in water – more specifically, Ti-oxide NPs spherically shaped. Initial results have shown that longer laser pulses have some advantage (NPs size peak at 100 nm, τ = 150 ps) compared to shorter pulses (NPs size peak 150 nm, τ = 40 ps).

    Center

    Center

    Periphery

    Periphery

    0

    mm

    mm

    2.013

    2.144

    Distance (mm)

    Hei

    ght

    (µm

    )

    +5

    0

    -5

    -10

    -15

    0.0 0.5 1.0 1.5 2.0

    mm

    mm

    0

    1.631

    1.566

    Distance (mm)H

    eigh

    t (µ

    m) +10

    0-10-20-30-40-50

    0.0 0.5 1.0 1.5

    Air

    Water