SEM MSE 421/521 Structural Characterization Historical Development 1935 - Knoll publishes the earliest known paper presenting the concept of a scanning electron microscope 1938 - Manfred von Ardenne constructs first STEM. First micrograph was of a ZnO crystal imaged at 23kV at a magnification of 8000x. The resolution was 50 - 100nm and took 20 min to record onto film. 1942 - First true SEM developed by Vladimir Kosmo Zworykin, J. Hiller, and R.L. Snyder at RCA Labs. The gun was at the bottom of the column! Resolution of about 50nm. Late 1940s - Charles Oatley at Cambridge selected Dennis McMullan to build an SEM as his PhD project – the SEM1. He placed the gun at the top of the column. 1947 - James Hiller patents the idea of using electrons to produce analytical x-rays (EDS), but he never constructs a working model 1952 - K.C.A. Smith develops method of detecting secondary electrons 1955 - T.E. Everhart develops what becomes the Everhart-Thornley detector 1961 - magnetic lenses are added for the SEM4 1965 - First four production models of the "Stereoscan" were delivered by Associated Electrical Industries http://www4.nau.edu/microanalysis/Microprobe-SEM/History.html MSE 421/521 Structural Characterization The Family of SEMs All SEMs have an electron gun, condenser, scanning coils, and a signal detection device Add EDS and possibly WDS it becomes an analytical SEM Hitachi 4500 SEM Add several WDS spectrometrs and it becomes a Microprobe (EPMA) MSE 421/521 Structural Characterization TEM SEM Electron gun Condenser system (2 lenses + 1 aperture) Scan coils Specimen stage Objective lens Objective aperture Scan generator Detector Principal image plane Monitor Projector lenses Viewing screen Vacuum system MSE 421/521 Structural Characterization SEM HT ~20 – 30 kV d ~ 2 – 10 nm Electron gun Scan generator Condenser lens Objective lens Aperture Scan coils Monitor Specimen stage Detector The objective lens in an SEM is really part of the condenser system, as it is not used for magnification but to demagnify the beam. Magnification involves NO lenses. MSE 421/521 Structural Characterization SEI Detector Everhart-Thornley detector Microscope chamber wall Faraday cage Electrons in Scintillator Light pipe Photomultiplier Electrical signal out Screen Quartz window +200 V +10 kV Always contains some back-scattered component Robinson detector – bulky, restricts WD, retracted for EDS MSE 421/521 Structural Characterization 100µ µm SEM Optics diameter of filament = d0 Strong C1 (small v1) means large u2 and small d. Apertures used to reduce spherical aberration I = I0(α1/α0)2 Physically fixed distance (v1 + u2) = constant demagnified source image diameter d1 at cross-over d1 = d0 x v1/u1 Minimised for large αo (strong C1) or small α1 (small objective aperture) final probe diameter d v1WD d = d1 x WD/u2 = d0 u1u2 ½A WD α tanα = A 2WD Can decrease probe size by either decreasing v1 and increasing u2 (increase strength of CL or increase V) or decreasing WD (increase strength of OL or increase V). ~α MSE 421/521 Structural Characterization SEM Performance Pixels (picture elements) ~ 100 µm, Specimen pixel size, p = 100 µm Resolution can never be better than p M Best to use a probe size, d, equal to p Probe size should be reduced as magnification increases. s = beam diameter defocus h = depth of field s=hα Assuming s ≤ p … s 100 µm h=α= Mα We already know that α ~ tanα ~ So, h = Can increase h by: WD 2WD (A) 100 µm 2WD M ½A A = α 0.2WD AM tanα = A 2WD ~α mm 1. Increasing WD - Degrades resolution 2. Decreasing size of objective aperture – May degrade resolution 3. Decreasing M MSE 421/521 Structural Characterization Resolution–Probe Size So, resolution is improved by: 1. Using a small λ (high kV)* 2. Using a large aperture (increasing α) – decreases h, increases Cc & Cs 3. Using a small probe current, i 4. Using a bright electron gun (typically FEG) We have already seen that I can be reduced by increasing the strength of C1 or decreasing WD; however, either increases spherical aberration (recall that rs = Csβ3). Minimum probe diameter for best resolution (d1 = 0) is: K ~ 1.22 Cs ~ 20 mm dopt = Kλ¾Cs¼ dopt ~ 2.3 nm (20 kV) As d decreases so does I. According to the Pease-Nixon equation: [ 3/8 ( ) + ]1 d = dopt 7.92x109 IT j I = probe current [A] T = temperature of filament [K] j = current density at filament surface [A/cm2] For thermionic emission MSE 421/521 Structural Characterization Resolution-Beam Current To resolve two points, there must be a visible difference in the signal generated from them. n = average number of electrons detected from a point, varies by ≤ C= n1 – n2 ∆n = (n1 > n2) n1 n1 n C = natural contrast (0 ≤ C ≤ 1) According to Rose, the eye can only distinguish between two adjacent points if n1 > n2 + 5 n1 (signal 1 is greater than signal 2 by five times the noise in signal 1) Minimum observable contrast level: C > n0 = It e = IF x 10-6 n = qn0 Ic > 4 x 10-12 qFC 2 [A] e 5 n1 n1 = 5 n1 n1 > 25 C2 n0 = number of electrons incident on a given pixel I = beam current t = time the beam stays at a given pixel F = entire frame scan time (assuming 1000x1000 pixels) n = number of electrons actually detected from a pixel q = constant related to detector efficiency and electron yield (0.1 < q < 0.2 for secondary electrons) Ic = critical current needed to see a contrast level C Actual contrast increases as n increases by: 1. Increasing beam current 2. Increasing scan time MSE 421/521 Structural Characterization Resolution = f(C) Resolution-Voltage photoresist on silicon MSE 421/521 Structural Characterization Topographical Images Kanter, 1961 δ= δ0 cosθ δ = Secondary electron coefficient δ0 = value of δ at normal incidence (θ = 0) Smallest for normal incidence (20° - 40° is common) Does not account for increased secondary electron emission caused by backscatter, which also increases with θ. δ Not valid for very low kV, in which case all secondary electrons escape Beam δ0 0 20 40 60 80 R θ Tilt (deg) MSE 421/521 Structural Characterization R0 θ Stereomicroscopy Two images are taken, one tilted 10-15° with respect to the other. Both are viewed simultaneously with a stereo viewer or anaglyph glasses. h= p 2Msin(θ/2) h = vertical height difference p = relative lateral displacement M = magnification θ = parallax angle Also possible (but highly unusual) to get topographical information using a small backscattered detector. - Only line-of-sight electrons detected, so emphasises shadows. - Modern BSI detectors are annular, so the effect is cancelled. MSE 421/521 Structural Characterization End of Lecture MSE 421/521 Structural Characterization