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01 e 03 de novembro Técnicas de Caracterização de Materiais – 4302504 2º Semestre de 2016 Instituto de Física Universidade de São Paulo Professores: Antonio Domingues dos Santos Manfredo H. Tabacniks Microscopias Caracterização dos Materiais Energia / Momento Matéria Propriedade a ser caracterizada Fótons Íons Átomos Elétrons Neutrons Prótons Fótons Íons Átomos Elétrons Neutrons Prótons Energia / Momento Matéria •Microscopias de Sonda Local (SPM) Nature Nanotechnology, 1 (2006) 3 + Caracterização dos Materiais Energia / Momento Matéria Propriedade a ser caracterizada Interação matéria- matéria, (ou radiação- matéria) Detectam- se forças ou corrente elétrica (ou intensidade luminosa) Energia / Momento Matéria •Microscopias de Sonda Local (SPM) Nature Nanotechnology, 1 (2006) 3 + Caracterização dos Materiais SPM Interação Ponta-Amostra Caracterização dos Materiais SPM Interação Ponta-Amostra Microscópio de tunelamento eletrônico (STM) Caracterização dos Materiais SPM Um pouco de história Heinrich Rohrer and Gerd K. Binnig, scientists at IBM's Zurich Research Laboratory in Switzerland, are awarded the 1986 Nobel Prize in physics for their work in scanning tunneling microscopy. Binnig and Rohrer were recognized for developing the powerful Scanning Tunneling Microscopy technique. They shared the award with German scientist Ernst Ruska, designer of the first Electron Microscope. US Pat. 4343993. IBM. J. Res. Dev. v.30, N4, 355 (1986) Experimental setup of first AFM from paper Binnig, Quate and Gerber (Phys.Rev.Lett.56,930 (1986)). Despite of the great success of the Scanning Tunneling Microscopy it was obvious that STM has fundamental disadvantage - with STM one can investigate only the conductive or conductive layers coated samples. This disadvantage was overcomed due to the invention of atomic force microscope by Binnig (US Pat. 4724318). He was first who have guessed that under interaction with sample surface macroscopic cantilever provided with sharp tip can be bended by atomic forces to sufficiently large amount to be measured by the common facilities. In first embodiment to measure tip displacement was used STM (Phys.Rev.Lett.56,1986,930-933). http://www.ntmdt.com/spm-principles/view/stm-techniques http://www.ntmdt.com/spm-principles/view/stm-techniques http://www.ntmdt.com/spm-principles/view/stm-techniques Caracterização dos Materiais SPM Um pouco de história Russell Young and his co-workers Fredric Scire and John Ward (left to right) with the Topografiner. It must be noted however that as long as in 1966 Russell Young has stated idea about an opportunity to acquire the surface topography with usage of current between surface and sharp metallic tip. In 1971 he have published paper about device called Topographiner, which contained all major assemblies of Scanning Probe Microscope. Phys. Rev. Lett. V. 27, N 14, 1971, P. 922-924 Rev. Sc. Instr. V. 43, N 7, 1972, P. 999-1011 Phys. Rev. Lett. 27, 922–924 (1971) Observation of Metal-Vacuum-Metal Tunneling, Field Emission, and the Transition Region Russell Young, John Ward, and Fred Scire National Bureau of Standards, Washington, D. C. 20234 Received 26 August 1971; published in the issue dated 4 October 1971 We report what we believe are the first observations of metal-vacuum-metal tunneling. A field emitter is brought close to a metal surface and the current-voltage characteristic is measured in three regions: the Fowler-Nordheim region, the intermediate region, and-and the metal-vacuum-metal region. © 1971 The American Physical Society URL: http://link.aps.org/doi/10.1103/PhysRevLett.27.922 DOI: 10.1103/PhysRevLett.27.922 http://publish.aps.org/search/field/author/Russell Young http://publish.aps.org/search/field/author/John Ward http://publish.aps.org/search/field/author/Fred Scire Caracterização dos Materiais SPM Interação Ponta-Amostra Microscópio de força atômica (AFM) Fig. 2 Schematic sketch of AFM from Patent "Atomic Force Microscope" (US RE37,299). For registration of cantilever bending many methods was used, but currently mostly useful and widely used is method invented by Amer and Meyer (see Fig. 2) US Pat. RE37,299 (Reissued Pat. No. 5,144,833) amostra magnética fibra óptica metalizada sistema de varrredura da amostra (XYZ) afinada e lock-in piezo-stack gerador de sinais diapasão bloco metálico laser Fotodiodo segmentado Diapasão de quartzo (tuning-fork) Caracterização dos Materiais SPM Interação Ponta-Amostra Microscópio de força atômica (AFM) Caracterização dos Materiais SPM Interação Ponta-Amostra Microscópio de força atômica (AFM) • Desenvolvemos uma nova unidade de AFM, operando no modo “tapping”. Neste caso o diapasão foi montado na horizontal. Para os testes iniciais, usamos pontas de tungstênio. Construímos as células eletroquímicas para a corrosão de fios de W e preparação da pontas. Pontas de tungstênio para AFM Microscópio de força atômica Imagem topográfica Imagem de erro Imagem de fase Nanopartículas de cobre Imagem topográfica Imagem de fase Caracterização dos Materiais SPM Interação Ponta-Amostra Microscópio de força atômica (AFM) • Scanning Probe Microscopies (SPM) Software Functions: - Control of the system - Image acquisition - Image processing Disponibility: - Software dedicated - WSXM from Nanotec - Open Source GXSM Software (Linux) Tip-sample distance control - Contact mode - Tapping mode - Shear-force mode Image construction - Feedback control signal - Direct measurement of any specific signal (amplitude or phase) - Retrace method • Scanning Probe Microscopies (SPM) Piezo-electric Scanner - Tube - Flexure - Bimorphes • Scanning Probe Microscopies (SPM) Feedback Control P I Signal Setpoint error Proportional Integral Z-piezo output Caracterização dos Materiais SPM Modo de Operação Microscópio de força atômica (AFM) - Modo de contato - Modo “tapping” (intermitente) ““ver simuladores”” Caracterização dos Materiais SPM Modo de Operação Microscópio de força atômica (AFM) - Força normal - Força lateral Microscópio de força magnética (MFM) Caracterização dos Materiais SPM Modo de Operação Microscópio de força atômica (AFM) - Força normal - Força lateral Caracterização dos Materiais SPM Microscópio de força atômica (AFM) Caracterização dos Materiais Nature Nanotechnology, 6 (2011) 191 SPM Comparação entre técnicas Microscópio ótico AFM MEV STM Caracterização dos Materiais SPM DME - Danish Micro Engineering A/S Herlev, Denmark PSIA Corp. Sungnam, Korea JPK Instruments AG Berlin, Germany QuantomiX Nes-Ziona, Israel NT-MDT, Molecular Devices and Tools for Nanotechnology, Moscow, Russia Quesant Instruments, Agoura Hills, CA Molecular Imaging Corporation, Phoenix, AZ. RHK Technology, Inc., Rochester Hills, MI Nanosurf AG, Liestal, Switzerland Surface Imaging Systems GmbH, Herzogenrath, Germany Nanotec Electronica Madrid, Spain Triple-O Microscopy GmbH, Potsdam, Germany Novascan Technologies, Inc. Ames, IA Veeco Metrology Group Woodbury, NY Omicron Vacuumphysik GmbH, Taunusstein, Germany Veeco Metrology Group was formed through the merger of Digital Instruments, Santa Barbara, CA and TM Microscopes, formerly ThermoMicroscopes, Inc., Sunnyvale, CA Merged brands also include Topometrix and Park Scientific Instruments. http://www.dme-spm.dk/ http://www.dme-spm.dk/ http://www.dme-spm.dk/ http://www.dme-spm.dk/ http://www.dme-spm.dk/ http://www.advancedspm.com/http://www.advancedspm.com/ http://www.advancedspm.com/ http://www.advancedspm.com/ http://www.jpk-instruments.de/ http://www.jpk-instruments.de/ http://www.jpk-instruments.de/ http://www.quantomix.com/ http://www.ntmdt.ru/ http://www.ntmdt.ru/ http://www.ntmdt.ru/ http://www.quesant.com/ http://www.molec.com/ http://www.rhk-tech.com/ http://www.nanosurf.com/ http://www.nanosurf.com/ http://www.nanosurf.com/ http://www.sis-gmbh.com/ http://www.nanotec.es/ http://www.nanotec.es/ http://www.nanotec.es/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.triple-o.de/ http://www.novascan.com/ http://www.novascan.com/ http://www.novascan.com/ http://www.veeco.com/ http://www.veeco.com/ http://www.veeco.com/ http://www.omicron.de/index2.html http://www.omicron.de/index2.html http://www.omicron.de/index2.html http://www.omicron.de/index2.html Using a form of atomic force microscopy, researchers can differentiate the chemical bonds in a single molecule of nanographene. [IBM)] Inventors reveal road to atomic force microscopy
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