Microscopia Eletrônica de Varredura e Nanoconformação com Feixe de Íons Marcos Vasconcellos Laboratório de Microanálise [email protected] www.if.ufrgs.br/~marcos PGCIMAT 2010 Jeol JIB 4500 Multbeam Http://nanolab.if.ufrgs.br Feixe de elétrons MEV Feixe de íons Ga Microscopia eletrönica de varredura - modo de elétrons secundários Supercondutores - monocristais em matrix policristalina Grupo de resistividade elétrica if-ufrgs Microscopia eletrönica de varredura - modo de elétrons secundários TiVAl - TiN Laboratório de Microanálise IF-UFRGS Microscopia eletrönica de varredura - modo de elétrons retroespalhados Pastilha de freio - filme de fricção Laboratório de Microanálise IF-UFRGS Silicon drift detector Detetor de raios X característicos 256 x 256 = 65536 x 1s = 18 horas!!!!!!! 256 x 256 = 65536 x 100 ms = 1,8 horas Al Ba Fe O O S Cu BSE C Modos de operação Imageamento desbastamento deposição Imagem de elétrons secundários Induzida por feixe de elétrons Induzida por feixe de íons Imagem de elétrons secundários Induzida por feixe de elétrons Induzida por feixe de íons Contraste de canalização do feixe de íons 15 20 25 FOCUSED ION BEAM 1. Equipamento a. sistema de vácuo b. liquid metal ion source – LMIS c. coluna iônica d. porta amostra e. detetores 2. Interação íon-sólido 3. Fontes de gás (deposição e remoção) 4. Sistemas dual beam 5. Imageamento 6. Nanofabricação 7. Preparação de amostras para TEM 8. Tomografia PGCIMAT 2010 1. Equipamento Diagrama b. fonte de íons liquid metal ion source (LMIS) Gallium (Ga) (i) its low melting point (T,, = 29.8 "C) minimizes any reaction or interdiffusion between the liquid and the tungsten needle substrate (ii) Its low volatility at the melting point conserves the supply of metal and yields a long source life; (iii) its low surface free energy promotes viscous behaviour on the (usually W) substrate; (iv) its low vapor pressure allows Ga to be used in its pure form instead of in the form of an alloy source and yields a long lifetime since the liquid will not evaporate (v) it has excellent mechanical, electrical, and vacuum properties, and (vi) its emission characteristics enable high angular intensity with a small energy spread. two step process: (i) The heated Ga flows and wets a W needle having a tip radius of - 2-5 pm. Once heated, the Ga may remain molten at ambient conditions for weeks due to its super-cooling properties. An electric field (lo8 Vlcm) applied to the end of the wetted tip causes the liquid Ga to form a point source on the order of 2-5 nm in diameter in the shape of a "Taylor cone." The conical shape forms as a result of the electrostatic and surface tension force balance that is set up due to the applied electric field. (ii) Once force balance is achieved, the cone tip is small enough such that the extraction voltage can pull Ga from the W tip and efficiently ionize it by field evaporation of the metal at the end of the Taylor cone. The current density of ions that may be extracted is on the order of - 1x10' ~ l cm*A. flow of Ga to the cone continuously replaces the evaporated ions c. coluna iônica F = q.E + q.v x B d. Stage X,y,z,R,Θ e. Detetores Elétrons secundários Elétrons retroepalhados EDS EBSD CL ... SDD MEV 2. Interação íon-sólido Regimes da cascata de colisões i) knock on regime MI << M2 ou E0 é baixo. ii) linear cascade regime FIB M1 ~ M2 iii) dense cascade regime M1 > M2 O mecanismo dominante de perda de energia no processamento com FIB (e.g., 5-50 keV) é o de interações elásticas entre o íon e os núcleos blindados (i.e., nuclear stopping). Conservação E e p Ziegler et al ZBL, LSS TRIM - SRIM http://www.srim.org/ TRIM calculation - Ga+ – 25 keV - 00 Flux is defined as the time rate of flow of energy; the radiant or luminous power in a beam. In the case of an ion beam flux is measured as the number of particles flowing through a given area per unit time and has units of ions/cm2/s. Fluence is, the sum of energies, the number of particles or photons incident during a given time interval on a small sphere centered at a given point in space divided by the cross-sectional area of that sphere. Fluence has units of ions/cm2 beam current is also a measure of the time rate flow of energy or how many ions are delivered per unit time. The beam current is measured in amperes, which is equivalent to units of charge per unit time or Coulombs(C)/sec. Current density is a measure of the energy intensity or number of ions in a given area at any instant in time. Current density has units of c/cm2 or in the case of a singly charged ion like ~ a t'hi s is equivalent to ions/cm2 http://www.srim.org/ 40 keV 5 keV sputtering 3. Imageamento Channeling contrast 4. Fontes de gás (deposição e remoção) varying dwell times 5. Sistemas dual beam 6. Nanofabricação Fabricação 3D 7. Preparação de amostras para TEM 0.5µm with a 13°taper angle 8. Tomografia Focused Ion-Beam Tomography A.J. KUBIS, G.J. SHIFLET, D.N. DUNN, and R. HULL METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 35A, JULY 2004—1935