2D-BLACK PHOSPHORUS FUNCTIONALIZED WITH METAL NANOPARTICLES: FULL CHARACTERIZATION AND CATALYTIC ACTIVITY ON HYDROGENATION REACTIONS
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1 2D-BLACK PHOSPHORUS FUNCTIONALIZED WITH METAL NANOPARTICLES: FULL CHARACTERIZATION AND CATALYTIC ACTIVITY ON HYDROGENATION REACTIONS EWPC-13 Freie Universität Berlin Salvatore Interlandi CNR-ICCOM Sesto Fiorentino (Florence)
2 Intro Outline 2D-black phosphorus (BP): a new wonder material 2D-BP as novel support for metal nanoparticles Experimental section Preparation and characterization of 2D-BP functionalized with TM nanoparticles Preliminary study on phenylacetylene hydrogenation catalyzed by NiNPs/2D-BP
3 Outline Intro 2D-black phosphorus (BP): a new wonder material 2D-BP as novel support for metal nanoparticles Experimental section Preparation and characterization of 2D-BP functionalized with TM nanoparticles Preliminary study on phenylacetylene hydrogenation catalyzed by NiNPs/2D-BP
4 2D-Materials Elemental 2D-materials 2D-Materials composed by two (or more) elements Graphene tride Molybdenum disulfide (MoS 2 ) Silicene.. Hexagonal boron nitride (h-bn)..
5 2D-Materials -Microelectronics -Optoelectronics -Catalysis -Chemical and biological sensors tride -Supercapacitors -Solar cells -Lithium ion batteries
6 Elemental 2D-Materials Isolated through exfoliation tride Graphene Other elemental 2Dmaterials Epitaxially grown onto specific substrates
7 2D-black phosphorus (BP): a new wonder material? Li, L.; Yu, Y.; Ye, G. J.; Chen, X. H.; Zhang, Y. Electronic Properties of Few-Layer Black Phosphorus. In APS March Meeting; American Physical Society: College Park, MD, 2013; abstract ID Most of the breakthroughs in this field are still to come. The Journal of Physical Chemistry Letters Perspective DOI: /acs.jpclett.5b01686 J. Phys. Chem. Lett. 2015, 6, BAPS.2013.MAR.J6.13, Session/J6.13.
8 2D-BP: a new wonder material?
9 Crystal structure of BP
10 Anisotropic structure of BP Zig-zag (y-axis)
11 Anisotropic structure of BP Armchair (x-axis)
12 2D-BP: highlights Semiconductor, with a thickness-dipendent direct band gap ( ev) Good carrier mobility ( 1000 cm 2 V -1 s -1 at room temperature) High surface area Higher chemical reactivity compared to other 2D-materials stable in free standing form - Careful handling in inert environments/encapsulation/passivation - Controllable/mild chemical functionalization (not possible for graphene)
13 2D-BP: highlights Semiconductor, with a thickness-dipendent direct band gap ( ev) -Communication -Light vision goggles -Thermal infrared imaging -Astronomy -Medicine -Document security systems -DVD players -Display -LED, OLED
14 2D-BP: highlights Semiconductor, with a thickness-dipendent direct band gap ( ev) Good carrier mobility ( 1000 cm 2 V -1 s -1 at room temperature) High surface area Higher chemical reactivity compared to other 2D-materials stable in free standing form - Careful handling in inert environments/encapsulation/passivation - Controllable/mild chemical functionalization (not possible for graphene)
15 2D-BP functionalization: a coordination approach? Reactivity towards soft Lewis acids: coordinatively unsatured TM complexes TM nanoparticles
16 2D-BP functionalization: a coordination approach? Reactivity towards soft Lewis acids: coordinatively unsatured TM complexes TM nanoparticles
17 Intro Outline 2D-black phosphorus (BP): a new wonder material 2D-BP as novel support for metal nanoparticles Experimental section Preparation and characterization of 2D-BP functionalized with TM nanoparticles Preliminary study on phenylacetylene hydrogenation catalyzed by NiNPs(TOP)/2D-BP
18 Preparation of 2D-BP Mechanical exfoliation PB 2D-BP Liquid phase exfoliation PB 2D-BP
19 Preparation of 2D-BP in our lab Prepared as described in: T. Nilges, M. Kersting, T. Pfeifer, J. Solid State Chem. 2008, 181, Exfoliation conditions as described in: M. Serrano-Ruiz, M. Caporali, A. Ienco, V. Piazza, S. Heun, M. Peruzzini, Adv, Mat. Interfaces 2015, 3,
20 Bright-field TEM image of 2D-BP M. Serrano-Ruiz, M. Caporali, A. Ienco, V. Piazza, S. Heun, M. Peruzzini, Adv, Mat. Interfaces 2015, 3,
21 AFM analysis of 2D-black phosphorus M. Serrano-Ruiz, M. Caporali, A. Ienco, V. Piazza, S. Heun, M. Peruzzini, Adv, Mat. Interfaces 2015, 3,
22 Extraction of 2D-BP from the DMSO of exfoliation
23 Preparation of NiNPs/2D-BP Prepared as described in: N. Mezailles et al. Nano Today 2012, 7, 21.
24 TEM image of NiNPs/2D-BP
25 Size distribution of NiNPs anchored on 2D-BP
26 EDX analysis of NiNPs/2D-BP
27 Number of Pd particles Preparation and TEM analysis of PdNPs/2D-BP Diameter (nm) Prepared as described in: Coronado et al. J. Mater. Chem. 2008, 18, 5682.
28 Number of Particles Preparation and TEM analysis of AuNPs/2D-BP Diameter (nm) Prepared as described in: Yang, J. Dong, Z. Yao, C. Shen, X. Shi, Y. Tian, S. Lin, X. Zhang, Sci. Rep. 2014, 4, 4501.
29 Number of Ru particles Preparation and TEM analysis of RuNPs/2D-BP Prepared as described in: H. Can, Ö. Metin, Appl. Cat. B-Environ. 2012, 125, Diameter (nm)
30 Intro Outline 2D-black phosphorus (BP): a new wonder material 2D-BP as novel support for metal nanoparticles Experimental section Preparation and characterization of 2D-BP functionalized with TM nanoparticles Preliminary study on phenylacetylene hydrogenation catalyzed by NiNPs/2D-BP
31 Phenylacetylene hydrogenation catalyzed by NiNPs Solvent Temperature ( C) Time (h) Conv. (%)* Selectivity toward styrene(%)* toluene toluene/dmso 1: toluene/dmso 1: * Evaluated by GC
32 Phenylacetylene hydrogenation catalyzed by NiNPs(TOP)/2D-BP Nicat = NiNPs Time (h) Conv. (%)* Selectivity toward styrene(%)* Nicat = NiNPs/2D-BP (P:Ni = 2) Time (h) Conv. (%)* Selectivity toward styrene(%)* * Evaluated by GC
33 Recycling the catalyst NiNPs/2D-BP n Conversion (%)* Selectivity towards styrene(%)* $ Catalyst was isolated by centrifugation (6000 rpm x 2 with acetone) before every recycling test * Evaluated by GC
34 Future work and perspectives Evaluate the effective heterogeneity of the studied catalytic system NiNPs/2D-BP (hot filtration tests, leaching tests ) and run a comparison of 2D-BP with other 2Dsupports for metal nanoparticles (graphene, carbon nanotubes ). Explore the catalytic activity of the other nanocomposites, RuNPs/2D-BP, PdNPs/2D-BP and AuNPs/2D-BP in several reactions. Clarify the nature and strenght of the interactions between TM nanoparticles and 2D-BP, using appropriate instrumental techniques (Raman, XPS spectroscopy...). Study the chemical and physical properties of the nanocomposites, in order to expand their uses in other fields (e. g. microelectronics, optoelectronics).
35 Intro Outline 2D-black phosphorus (BP): a new wonder material 2D-BP as novel support for metal nanoparticles Experimental section Preparation and characterization of 2D-BP functionalized with TM nanoparticles Preliminary study on phenylacetylene hydrogenation catalyzed by NiNPs/2D-BP
36 Acknowledgements CNR-ICCOM: -Maria Caporali -Maurizio Peruzzini -Manuel Serrano Ruiz -Matteo Ceppatelli -Andrea Ienco -Gabriele Manca CNR-IMM: -Giuseppe Nicotra CNR-NANO: -Stefan Heun -Francesca Telesio -Shaohua Xiang The authors thank the European Research Council for funding the project PHOSFUN Phosphorene functionalization: a new platform for advanced multifunctional materials (Grant Agreement No ) through an ERC Advanced Grant to MP.
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