Andromeda and END-MS, New generation of Surface Analysis Instrument

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1 Andromeda and END-MS, New generation of Surface Analysis Instrument S. Della-Negra (1),E. Cottereau (1), V. Huc (2), B. Rasser (3) and E.A. Schweikert (4) (1) Institut de Physique Nucléaire d Orsay, UMR 8608, Université Paris Sud, F91406 Orsay Cedex (2) Institut de Chimie Moléculaire et des Matériaux d Orsay, UMR 8182, Uni. Paris-Sud 11, F91405 Orsay (3) OrsayPhysics, ZA Saint Charles, F13710 FUVEAU (4) Centre for Chemical Characterization and Analysis, Texas A&M Univ., College Station, TX For a few years the collaboration between our groups explored the advantages of Nano- Particle (NP) projectiles for the surface analysis. Our studies led to the Pegase project, founded by NSF (Grant CHE ) and installed in TAMU, which allows a 130 KV acceleration of NPs delivered by a LMIS source (Liquid Metal Ion Source). The Pegase instrument is working with success since one year and a half. The first results presented during this conference demonstrate the interest of this new probe for the biological and also nano-structured surface analysis. The Pegase project allowed the design of new more ambitious instruments taking into account the results obtained at higher energies in the MeV range [2] named ANDROMEDA and END-MS (Environmental Nano domain-mass Spectrometry). The differences between the two projects are the energy, respectively 4 MV and 1 MV and the framework respectively national facility and university facility. At the beginning of this year, Andromeda has won the national call for proposal EQUIPEX (Excellence Equipment) and the realization is starting. The goal and therefore the heart of the two projects are the same: The goal is to create a new instrument for the analysis by mass spectrometry of nanofields and nano-objects present on a surface with a spatial resolution of ~100 nm. This instrument is also meant for the surface analysis at the ambient pressure and therefore the mass spectrometry analysis on native hydrated biological surfaces. Molecular information (mass and structure) will be obtained from the impact of a Nano-Particle accelerated in the MeV range by a Van de Graaff electrostatic accelerator from 1 to 4 MV. The principal devices of the new instrument are a rising generation of ion sources NAPIS (NAno Particle Ion Source), the accelerator and the localization of the impacts of NPs to reach nanometre dimensions; this last point was developed by the TAMU group[3]. The dedicated instruments installed will be a ToF mass spectrometer with high mass resolution, and finally the bombardment at the quasi-ambient pressure associated to an effective analysis by mass spectrometry. We shall recall the main results leading to the new projects. The projects will be described and the first results concerning the source R&D in progress will be presented: metallic nanodroplet beam provided by a commercial FIB (Focussed Ion Beam) column COBRA X from OrsayPhysics and preparation of the new NAno-Particles Ion Source (NAPIS). The Pegase project, a new solid surface probe: focussed massive cluster ion beams S. Della-Negra, J. Arianer, J. Depauw, S.V. Verkhoturov and E.A. Schweikert, Surf. Interface Anal.,2011, 43, [2] Massive Clusters: Secondary emission from qkev to qmev. New emission processes? New SIMS Probe? S. Della-Negra, J. Depauw, C. Guillermier and E.A. Schweikert, Surf. Interface Anal.,2011, 43, [3] Single Impacts of C 60 on Solids: Emission of Electrons, Ions and Prospects for Surface Mapping. S. Verkhoturov, M. Eller, R. Rickman, S. Della-Negra, E.A. Schweikert. J. Phys. Chem. C, 2010, 114 (12), pp

, College Station, TX 77843-3144 For a few years the collaboration between our groups explored the advantages of Nano- Particle (NP) projectiles for the surface analysis.

2 ANDROMEDE AND END-MS, NEW GENERATION OF 18 septembre 2011 SURFACE ANALYSIS INSTRUMENT S. Della-Negra 1, E. Cottereau 1,V. Huc 2, B. Rasser 3 and E.A.S. Schweikert 4 1 Institut de Physique Nucléaire d Orsay, UMR 8608, Université Paris Sud, F91406 Orsay Cedex 2 Institut de Chimie Moléculaire et des Matériaux d Orsay, UMR 8182, Uni. Paris-Sud 11, F91405 Orsay 3 OrsayPhysics, ZA Saint Charles, F13710 FUVEAU Unité mixte de recherche CNRS-IN2P3 Université Paris-Sud Orsay cedex Tél. : Fax : Centre for Chemical Characterization and Analysis, Texas A&M Univ., College Station, TX dellaneg@ipno.in2p3.fr 1

3 ANDROMEDE R&D LMIS kev Au n C 60 MeV 3 accelerators TAMU Au nq q+ n>40 to 1000 Pegase Impact Secondary Giant Enhancement Orthogonal Metal of slow time ion Sputtering Secondary gold of flight emission clusters Yields Ion secondary Emission under cluster Induced various ion impact by solids. under mass Gold spectrometry at Non low kev/atom Cluster linear effects Bombardment analysis energy (5-60 Gold in kev), Cluster secondary of peptides with ion Energy using influence of the emission, Secondary ion yields from surfaces bombarded with kev molecular and cluster ions, number H.H. from large ANDERSEN, kev gold to clusters MeV per as of atoms in A. primary the BRUNELLE, atom. ions projectiles, S. DELLA-NEGRA, J. DEPAUW, D. JACQUET, Y. M. LE S. A. AGNÈS DELLA-NEGRA, BENGUERBA, A. H. BRUNELLE, JORET, Y. LE S. BEYEC, M. BLAIN J. and E.A. SCHWEIKERT, K. BEYEC, BRUNELLE, TEMPEZ, BOUSSOFIANE-BAUDIN, J. CHAUMONT, S. J.A. DELLA-NEGRA, SCHULTZ, H. G. BERNAS S. DELLA-NEGRA, J. DEPAUW, D. JACQUET, J. DEPAUW, Y. LEBEYEC, BOLBACH, A. BRUNELLE, S. DELLA-NEGRA, H. D. JORET, JACQUET, Y. M. LE A. J. BEYEC, PAUTRAT, NOVIKOV, DEPAUW, Phys. Rev. M.G. K. Y. P. HAKANSSON BLAIN, BAUDIN, LEBEYEC, Lett. Letters 80 E.A. H.H. M. (1998) SCHWEIKERT, PAUTRAT, ANDERSENM. and 63, Y LE BEYE (1989) G. CAROFF, BEN ASSAYAG, M. UGAROV, P. SUDRAUD, H. BENSAOULA, M. GONIN, K. FUHRER, AND AMINA WOODS Phys. Nucl. Rev. Instr. A and 63 Meth. (2001) B Rapid Communications in Mass (1994) Spectrometry, , (2004) Nucl. Instr. and Meth. B62 (1991) 8. 2

under mass 20-5000 Gold spectrometry at Non low kev/atom Cluster linear effects Bombardment analysis energy (5-60 Gold in kev), Cluster secondary of peptides with ion Energy using influence of the

4 ANDROMEDE CN - (M-H) - (M 2 -H) - - AuCN 2 13 C 15 N Counts Absolute Yield Single impact Au q+ 450 qkev 2 0,1 Au 100q q Energy 3350per charge 3400 (kev/q) Time (0.8 ns/channel) 3

450 qkev 2 0,1 Au 100q q+ 0 10 100 1000 3250 3300 Energy

5 ANDROMEDE The goal of Andromeda is to create a new instrument for the analysis by mass spectrometry of nano-fields and nano-objects present on a surface with a spatial resolution of ~ 500 nm. Moreover this instrument will permit the surface analysis at the ambient pressure and therefore the mass spectrometry analysis of native hydrated biological surfaces. This project is a very efficient alternative to the Secondary Ion Mass Spectrometry, SIMS. Molecular information (mass and structure) will be obtained starting from the impact of a Nano-Particle accelerated in the MeV field by a Van De Graaff electrostatic accelerator from 1 to 4 MV 4

Moreover this instrument will permit the surface analysis at the ambient pressure and therefore the mass spectrometry analysis of native hydrated biological

6 ANDROMEDE NAPIS ECR 5

incorporated in a conducting solid polymer, which can melt

7 ANDROMEDE - NAPIS Mono-dispersed Pt nano-particles produced by chemists The LMIS design is possible with NPs incorporated in a conducting solid polymer, which can melt by heating LMIS >>>> NAPIS Collaboration with ICMMO and Orsayphysics 6

8 ANDROMEDE ECR ION SOURCE C 60 + C C Magnet Current I (au) 7

9 ANDROMEDE 8

10 ANDROMEDE COBRA X 9

11 ANDROMEDE COBRA X Au + Au + Ge ++ Ge + Au ++ AuGe + Au 2 + Au 3 + Au 100q q+ Au q+ 33q Au q+ Au q+ 61q 100q Energy = 30 kv, emission = 20 & 40 µa, probe aperture = 800 µm, mass aperture = 50 µm Heavy gold cluster beams production and identification S. BOUNEAU, S. DELLA-NEGRA, J. DEPAUW, D. JACQUET, Y. LEBEYEC, J.P. MOUFFRON, A. NOVIKOV, M. PAUTRAT. N.I.M. B225 (2004)

50 µm Heavy gold cluster beams production and identification S. BOUNEAU, S. DELLA-NEGRA, J.

12 ANDROMEDE COBRA X AuGe 11

13 Counts ANDROMEDE COBRA X Bi Bi 100q q+ [ClBr-Br - ] [142] + 60 Counts 40 [Trifluo-2HCl] Channel 1000 Bi Channel 12

[Trifluo-2HCl] + 20 2000 0 6000 6300 6600

14 ANDROMEDE COBRA X Bi Clidinium Bromide (2.5mg) et Trifluoperazine (1mg): Fludininium Yield enhancement Ratio Bi + Bi + 2 Bi + 3 Bi 2+ 3 Bi 2+ 5 Bi 100 [ClBr-Br - ] + / [Trifluo-2HCl] & Internal energy transfer decrease 13

15 THANK YOU FOR YOUR ATTENTION 18 septembre 2011 Unité mixte de recherche CNRS-IN2P3 Université Paris-Sud Orsay cedex Tél. : Fax : This work has benefited from government aid administered by the National Agency for Research under the program for future investment (Equipex). 14

: +33 1 69 15 73 40 Fax : +33 1 69 15 64 70 http://ipnweb.in2p3.

Imagerie biologique par spectrométrie de masse TOF-SIMS et MALDI-TOF

Imagerie biologique par spectrométrie de masse TF-SIMS et MALDI-TF 12 juin 212 Alain BRUNELLE Centre de recherche de Gif Institut de Chimie des Substances Naturelles Gif-sur-Yvette France Alain.Brunelle@icsn.cnrs-gif.fr