透射电镜样品的备干粉法 液体.ppt

倒易点阵与正点阵 衍射几何条件：厄瓦球面 The size of diffraction patterns (1/l)/ghkl＝L/Rhkl’ R’d = lL When is q small (electron diffraction), Rd=lL=diffraction constant Plotting and indexing of single crystal spot patterns When q is small (electron diffraction), the reflection sphere cuts a 2D reciprocal plane. Plotting and indexing of single crystal spot patterns Indexing: the plane normal [uvw] and at least one low index spot (hkl) (normally two spots), with hu+kv+lw=0. Plotting and indexing of single crystal spot patterns For a known substance but unknown orientation, a table of interplanar spacings d is needed. a) Choose three spots such as h3k3l3, h1k1l1, h2k2l2. b) Measure the d values, and thus determine the indices. c) By trial and error a consistent set of indices is chosen such that h3k3l3= h1k1l1 + h2k2l2. d) [uvw], the zone axis, is obtained by any two vectors (e.g. R1×R2) Plotting and indexing of single crystal spot patterns Example: an fcc crystal with a = 0.58nm. d=a/(h2 +k2 +l2)1/2. A diffraction pattern is shown below with R1=R2=8.96mm, R1^R2=109.5o. Ll=3.0 nm.mm. a) Choose three spots R1, R2, R3 (R3 = R1 + R2 ) b) d1= d2= Ll/R1= 0.335nm, ? {111}. c) A consistent set of indices is 002= 111 + -1-11. d) R1×R2=[1-10], the zone axis晶带轴. Indexing of single crystal spot patterns from an unknown phase Procedure Survey the literature to collect information of possible phases. Three possible routes to reach its full indexing Calculate d spacings and compare with standard powder XRD data; Measure R2/R1, R2^R1, and compare with tables in archives; Try a cubic phase; Use double tilting to determine directly the 3D reciprocal lattice. In general three independent patterns are necessary to determine a reciprocal structure. Standard powder XRD data; Cubic indexing Cubic indexing Choose three shortest reciprocal vectors R1, R2, R3, R3=R1+R2, measure the angle R1^R2. Calculate d1, d2, (R2/R1)2, (R3/R1)2. Judge possible combinations of hkl. In general three independent p