Solutions of Chapter 3 3.1. Generally, the wavelength of electron and the acceleration voltage has a relation as λ ∝ 1/ Vo . Do the values in Table 3.2 hold the relation exactly? Show the relations between λ and Vo in Table 3.2 and comparing them with λ ∝ 1/ Vo . The wavelength of electron λ is determined by its velocity v and mass m,that is h (1.1) λ= mv Where h is Planck’s constant. While the velocity v and the acceleration voltage has the following relation, 1 2 mv = eV 2 We obtain v= 2eV m (1.2) From equation (1.1) and (1.2), we can get λ = h h = / V0 2emV 2em If the velocity of electron is relatively low, its mass is almost equal to the static mass. That is m= m0 . If the velocity of electron is very high, it should be rectified m0 by theory of relativity. m = 2 ⎛v⎞ 1− ⎜ ⎟ ⎝c⎠ We know Planck’s constant h = 6.63 × 10-34 J − s , e = 1.602 ×10-19 C . Supposing m = m0 = 9.11× 10-31 kg ; thus h 6.63 ×10-34 = = 1.22718 × 10-9 . -19 -31 2em 2 ×1.602 × 10 × 9.11×10 We can calculate the correlations and compare them with Table 3.2, as shown in the following table. Acceleration voltage (KV) 40 60 80 100 200 500 Electron wavelength (nm) 0.00614 0.00501 0.00434 0.00388 0.00274 0.00174 Electron wavelength(nm) in Table3.2 0.00601 0.00487 0.00418 0.00370 0.00251 0.00142 Materials Characterization Yang Leng © 2008 John Wiley & Sons (Asia) Pte Ltd 1 From the comparison, we can find that the wavelength values are slightly shorter due to the consideration of the relativity theory. 3.2. The resolution of TEM is limited by the diffraction (Rd) as discussed in Chapter I (Eq. 1.3) and by the spherical aberration which is expressed as Rsph = Csα 3 . The TEM resolutions are the quadratic sum of diffraction and spherical aberration one ( R = Rd 2 + Rsph 2 ). The minimum R is obtained when Rd ≅ Rsph. Estimate the optimum value of α and resolution limit of TEM at 100 and 200 kV. Cs ≅ 1 mm for an electromagnetic objective lens. With α decreasing, the spherical aberration will decrease but the resolution will be worse. Considering the diffraction limited resolution and spherical aberration, the optimum value of α can be obtained as follows. 0.61λ , Since Csα 3 = μ sin α 1 ⎛ 0.61λ ⎞ 4 we get α = ⎜ ⎟ . ⎝ μ Cs ⎠ At 100KV, as is shown in table 3.2, the corresponding electron wavelength is 0.00370nm. For Cs ≅ 1mm and supposing μ ≈ 1 , we can estimate α = 6.228 ×10−3 , and the resolution R1 = 0.61λ 0.61× 0.0037 nm = = 0.362nm μ sin α 1× 6.228 ×10−3 Similarly, for 200KV; we can get α = 5.652 × 10−3 and R1 == 0.61× 0.00251nm = 0.275nm 1× 5.565 ×10−3 3.3. How to increase contrast of mass-density image? Explain why. Can we obtain a mass-density image of metal specimen? Can we obtain a diffraction contrast of a polymer specimen? Staining with solution with heavy metal elements is common method used to increase contrast of polymeric and biological specimens. Heavy metal ions may selectively stain certain constituents in the specimens, and thus increase the mass-density among different constituents. The staining method does not work well with metal. However, the mass-contrast exhibits in all types of materials, including metals. Generally, the diffraction contrast does not work well in a polymer specimen because only crystalline polymer may generate diffraction contrast. 3.4. Note that both the mass-density and the diffraction contrast requires only transmitted beam pass the objective aperture. How can you possibly know you have a diffraction contrast without checking SAD? Materials Characterization Yang Leng © 2008 John Wiley & Sons (Asia) Pte Ltd 2 The diffraction contrast is very sensitive to specimen tilting, but mass-density is not. We may tilt the specimen and check whether the contrast of the image changes during tilting specimen. 3.5. Sketch diffraction patterns of single crystals in TEM: a) FCC crystal with transmitted beam direction (B) parallel to [001]; b) BCC crystal with B = [001]. This question should have same answers as questions 2.5 and 2.6. (BCC) (FCC) 3.6. Does a zone axis of single crystal diffraction is exactly parallel to transmitted beam? Explain your answer graphically. To obtain a single crystal diffraction pattern, it is not necessary to have a zone axis exactly parallel to transmitted beam. As shown in the above figure, the zone axis is not exactly parallel to the transmitted beam. Due to thin foil effect, the reciprocal point will extend to rod, if the Edwald sphere cut the rod, we can also get diffraction pattern of single crystal. Materials Characterization Yang Leng © 2008 John Wiley & Sons (Asia) Pte Ltd 3 3.7. What kind of diffraction patterns you should expect, if a SAD includes a large number of grains in a polycrystalline specimen? Why? A ring pattern will be as shown in Fig. 3.34a. The pattern including a large number of grains, which randomly orientated in the specimen, is equivalent to rotate a single crystal pattern along axis perpendicular to the image plane. 3.8. You are asked to obtain maximum contrast of one grain from its neighbors. Which orientation of crystalline specimen do you wish to obtain? Illustrate it with a pattern of single crystal diffraction. The orientation of the specimen should let one set of crystallographic planes in the grain satisfies the exact Bragg’s condition. It means that the intensity of such diffraction is maximized. In such case, the dark image of the grain distinguish itself with surround ones. 3.9. You have been told that thickness fringe and bend contours can be distinguished How? Thickness fringes often show as a pattern with rather regularly spacing between bright and dark fringes. Bend contours do not show much regularity in the fringe spacing. The bend contours are sensitive to specimen titling, but not the thickness fringes. 3.10. The reason we see a dislocation is that it bents crystal plane near its core region. Can you indicate a case we may not be able to see the dislocation in diffraction contrast in a two-beam condition (the two-beam condition is referred to a crystal orientation in which intensity of one diffract spot is much higher than those of rest spots)? Please indicate the either graphically or using the relation of vectors g (normal of planes which generate the diffraction beam) and b (Burgers vector of dislocation). The dislocation contrast can disappear if g hkl ⋅ b = 0 , the dislocations will be invisible. In other word, when g ⊥ b, we can not see the dislocation. Materials Characterization Yang Leng © 2008 John Wiley & Sons (Asia) Pte Ltd 4
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