Lecture 2 Basic alignment & Electron material interaction Bo Zhao 2014 Fall semester Quick review for last lecture FESEM gun source—how electrons are generated Electromagnetic lenses, apertures—define a fine beam Deflection coils—direct the beam onto different locations Sample stage—move your sample around and grounding Are you still a treasure hunter? Electron Gun Candle Apertures Condenser lens Hand Deflection or Raster coils Objective lens Map Sample Eyes Detectors Brain/memory Viewing screen/camera 3 How can we make the image better? Spot size Users define the resolution---------spot size! 4 Two main goals Focus a small beam of electrons onto the sample ------- alignment Detect products of beam/sample interaction -------- signal generation and collection Components e- Basic assembly in Hitachi S4300 Condenser lens Main role: Concentrate the electron beam Affect the spot size Objective lens Main role: focusing the beam onto the sample Has some influence over the diameter of the spot size Note: a focused beam produces a smaller spot on the sample surface than an under or over-focused beam Basic Alignment Alignment steps goes from top to bottom Beam alignment Aperture alignment Stig X, Stig Y alignment On the Instrument We have learned how to load the sample into the S.C., so let’s continue…. Basic info the instrument needs to know Sample size--- sets limits of sample stage movement in XY direction Working distance Accelerating voltage--- depends on your sample and what info needs to be obtained from the sample Gun brightness--- the flow of electrons emitted by the filament h Properties of Electron beam • Gun Brightness defined as beam current density per unit solid angle. 12 Vacc: 1 KV Gun brightness:1 Vacc: 10 KV Gun brightness:1 Vacc: 1 KV Gun brightness:2 Understand the difference between Vacc and Ie Accelerating Voltage ----how fast an electron travels--- --How much energy it carries---- knock out different signals Emission Current----how many electrons travels per second-----how many bombard your sample per second----signal Turn on the HV SOP 2.2 Find an image 2.2.1 Setup the high voltage and click on. 2.2.2 Adjust the image magnification couterclockwise. Click ABC to auto adjust brightness and contrast. Use the Trackball to move the sample to the area of interest. 2.2.3 Sharpen image and adjust the brightness and contrast using the Focus, Brightness, and Contrast rotary controls. SOP 2.3 Alignment 2.3.1 Click on the aperture option and center the aperture by click the reset button at the bottom right corner. Pull the objective aperture out to “0”position. 2.3.2 Click on the beam. Center the beam position. Then insert the objective aperture. If no beam is visible, crank up the contrast and brightness until you can observe beam light, then center the beam. 2.3.2 Click on the aperture option again, adjust the two knobs on the objective aperture on the column unit to stop the image fluctuation. 2.3.3 Click on the stigma X, adjust the X,Y knobs on the control panel to stop the image shift in any direction. 2.3.4 Click on the stigma Y, adjust the X,Y knobs on the control panel to stop the image shift in any direction. 2.3.5 Click on “off ” to stop the alignment procedure. Reset Aperture is out, aperture settings are reset Center the beam Choose the beam option, center the beam by using the X,Y knobs for alignment on the control panel Put in the objective aperture Position to the desired aperture number and then center the beam by adjusting the two knobs on the aperture e - e - e - Aperture Alignment No aperture Good aperture alignment Bad aperture alignment Mechanically align the aperture Top view Side view Fine alignment of aperture You will see the image shifting back and forth, stop the movement by tuning the aperture knobs (one at a time!) until the image stop moving Wobbler Stig X Stig Y Align stig X and Stig Y Stop the imaging shifting by using the two alignment X Y knobs on the control panel. Stigmatic Aberration This defect is the result of the demagnification of the condenser lenses in one direction being greater than the demagnification in another direction Wobbler Off Switch back to the image and then focus Questions? Sputter coating Reduced electron beam damage. Increased thermal conduction. Reduced sample charging (increased conductivity) Improved secondary electron emission Reduced beam penetration with improved edge resolution Protects beam sensitive specimens Mechanism When a target is bombarded with fast heavy particles, erosion of the target material occurs. Control panel Beam material interaction SEM techniques SE BSE EDX Cathodoluminescence STEM Electron beam-sample interactions The incident electron beam is scattered in the sample, both elastically and inelastically This gives rise to various signals that we can detect (more on that on next slide) Interaction volume increases with increasing acceleration voltage and decreases with increasing atomic number Signals from the sample Incoming electrons Secondary electrons Auger electrons Backscattered electrons Cathodoluminescence (light) X-rays Sample What information does scanning electron microscope provide us? surface morphology Phase distribution Elemental composition Defects, impurities 41 http://mee-inc.com/sem.html Macroscopic view Electron beam shooting on your sample, no matter how conductive your sample is, it will have resistance, so there will be heat generated, and it is the major damage cause Microscopic view particle collision theory Inelastic collision when it lost energy, in what form that energy has changed into? heat? Other form? Elastic collinsion small or no energy loss, opposite direction Remember Electron has particle wave duality? Particle Collision Inelastic Secondary electron, X-ray Elastic backscattered electron Secondary electrons (SE) Low energy electrons (~10-50 eV) Only SE generated close to surface escape (topographic information is obtained) High resolution Uniformity SEM images of 1500/110 nm “raspberry-like” templates and bimodal porous gold electrode 45 •Bo Zhao, Maryanne M. Collinson, Chemistry of Materials 2010, 22(14), 4312-4319. Edge effects 46 Backscattered electrons (BSE) A fraction of the incident electrons is retarded by the electro- magnetic field of the nucleus and if the scattering angle is greater than 180 ° the electron can escape from the surface SE MENA3100 BSE How many electrons got returned determine the signal Nuleus is a “particle” too, if the positive charge on it is strong, it has more influence on the electrons, Note: what determine the charge? proton number, which is also Z value, atomic number When the atomic number is high, the atomic size is small, which means that they are more compact. Distribution of reinforcement phase in matrix and their bonding (a) (b) (a) W80Al20/90Ni-5Fe-5Mo (b) back scattering image of (a) 49 •B. Zhao, C.J. Zhu, X.F. Ma, W. Zhao, H.G. Tang, S.G. Cai, Z.H.Qiao, Materials Science & Engineering A 456, 2007, 337-344. EDX spectroscopy Emission energy is “characteristic” of energy level differences Each element has a fingerprint X-ray signal 50 SEM electron (e.g. 20 keV) “kicks out” electron from “K-shell” EDX-qualitative and quantitative analysis Y: 79.4% Yb: 19.3% Er: 1.3% Characteristic x-rays Continuum, Bremsstrahlung 3+,SEM Top) Powder XRD pattern :and (bottom) image of3+NaYF4:2%Er, NaYF 3%Er 17%Yb 4 le from Lorad Chemical Co. The XRD pattern is compared to ICCD for hexagonal Consideration () phase NaYF4. The crystallites are phase-pure and cron size range. Dead time 51 For quantitative analysis, standard is required Statistics: Signal-to-noise ratio Drift in electron beam with time Build-up of a carbonaceous contamination film after extended periods of electron probe irradiation Elemental mapping Mapping Allows selection of elements to be mapped Shows spatial distribution of elements in sample Meteorite sample Fe Mo Ni Ca Mg 52 http://microanalyst.mikroanalytik.de/info7.phtml
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