Modern Powder Diffraction

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Page 1 Titles , I REVIEWS in MINERALOGY Volume 20 MODERN D.L. BISH AND J.E. POST, editors Authors: Series Editor: Page 1 Page 1 Titles Reviews in Mineralogy Volume 20 MODERN POWDER DIFFRACTION Page 2 Page 1 Page 2 Page 3 Page 4 Titles Chapter 6 R. C. Reynolds, Jr. DIFFRACTION BY SMALL AND DISORDERED CRYSTALS Chapter 7 D. K. Smith COMPUTER ANALYSIS OF DIFFRACTION DATA 185 PDF-1 186 PDF-2 186 PDF-3 Page 5 Page 6 Page 7 Page 8 Page 1 Page 2 Titles 2 Page 3 Titles 3 o 30 Page 4 Titles 4 Page 5 Titles 5 Page 6 Titles 6 Page 7 Titles CuKa 29 o _p=4ooA 7 B I Page 8 Titles 8 Page 9 Titles 9 (10) Page 10 Titles 10 Page 11 Titles F(OOI ) = L nj fj cos(21t1 Zj Ie) , 11 Page 12 Titles 12 I(hkl) = Lp(S) IF(hkl ~ 2 sin2(1th Nl) sin2(1tk N2) sin2(1t1 N3) Page 13 Titles 13 Page 14 Titles 14 Page 15 Titles -k tb lie 012 022 100 h fa 122 \;ii') 15 -kfb 30 32 34 36 38 029 Page 16 Titles 16 I = (c/d> sin 'Y. Page 17 Titles 17 Page 18 Page 1 Titles 2. INSTRUMENT A TION Ron Jenkins (1) Page 2 Page 3 Page 4 Titles 22 ~ , \ '(~J' Page 5 Titles 23 Page 6 Titles 24 Page 7 Page 8 Titles 26 • -------- -' -------------------------------- Page 9 Titles 27 Page 10 Titles I ~ 60 610 28 Tables Table 1 Table 2 Page 11 Page 12 Titles 30 i " o Tables Table 1 Page 13 Titles 31 Page 14 Titles 32 Page 15 Titles 33 Tables Table 1 Page 16 Titles 34 Page 17 Titles 35 Page 18 Page 19 Titles 3 Fluorescence Type 2 Scatter f ~ Source e Gives d c 37 a b c CoKClt HI KCl t CoKCl2 HI KCl2 7.5 a.o 1.5 t.O Page 20 Titles 38 Page 21 Titles 39 Page 22 Titles 40 Tables Table 1 Page 23 Titles 41 Tables Table 1 Page 24 Titles 42 :E"' --- -----T M Page 25 Titles 43 Page 26 Titles 44 Page 27 Titles 45 Page 28 Page 1 Titles 3. EXPERIMENTAL PROCEDURES Ron Jenkins Page 2 Titles 48 cis 3.0 100l Tables Table 1 Page 3 Titles 49 Page 4 Titles 50 Page 5 Titles 51 cIs 60 ----- -------- Tables Table 1 Page 6 Page 7 Titles 0-'" 53 ~ f )+-( Page 8 Titles 54 Page 9 Titles _jl_'8 55 Page 10 Titles 56 Page 11 Titles 57 Page 12 Titles 6. • • • 7. a) J;:l Tables Table 1 Page 13 Titles 59 ~ J\ .. 29 V Tables Table 1 Page 14 Titles 60 Page 15 Tables Table 1 Table 2 Page 16 Titles 62 L\dld = -L\E> cotE> . (5) Page 17 Titles 63 Page 18 Titles 64 Table 8. Factors affecting X-ray powder diffraction line intensities. 1) Structure Sensitive - Atomic scattering factor - Structure factor - Polarization - Multiplicity - Temperature 2) Instrument Sensitive a) Absolute intensities - Source intensity - Diffractometer efficiency - Take-off an~e of tube - Receiving slit width - Axial divergence allowed b) Relative intensities - Divergence slit aperture - Detector dead-time 3) Sample Sensitive - Crystallite size - Degree of crystallinity - Particle orientation 4) Measurement Sensitive - Method of peak area measurement - Method of background subtraction - 0:2 stripping or not - Degree of data smoothing employed Tables Table 1 Page 19 Titles 65 Page 20 Tables Table 1 Page 21 Titles 67 Page 22 Titles 68 Page 23 Titles 69 Page 24 Titles 70 Page 25 Titles 71 Page 26 Page 1 Titles 4. SAMPLE PREPARATION FOR X-RAY DIFFRACTION Page 2 Titles 74 Page 3 Titles 75 Page 4 Titles 76 Page 5 Titles 77 Page 6 Titles 78 Page 7 Titles 79 Page 8 Titles 80 _ KLp(9)IF(hkl)12 I(hkl) Page 9 Titles v 81 Page 10 Titles 82 Page 11 Titles 83 Page 12 Titles 84 Page 13 Titles 85 Page 14 Titles 86 °28 (CuKa) Page 15 Titles 87 Page 16 Titles 88 Page 17 Titles 89 Page 18 Titles 90 Page 19 Titles 91 Page 20 Titles 92 Page 21 Titles 93 Page 22 Titles 94 Page 23 Titles °28 (CuKa) 60 Z 40 o o 20 °28 (CuKa) 50 44 38 32 26 20 14 8 o 160 o 120 x ~ 80 Z ::> o o 40 °28 (CuKa) Tables Table 1 Page 24 Titles 96 Page 25 Titles 97 Page 26 Titles 98 Page 27 Titles 99 Page 28 Page 1 Titles 5. QUANTITATIVE ANALYSIS Page 2 Titles 102 (1) Page 3 Titles 103 (2) Page 4 Titles 104 (3) ,. X: = 1- X .. (4) (5) Page 5 Titles 105 (6) Page 6 Titles 106 I/Ieorundum Page 7 Titles 107 t.; Ij~' x, t.; Ij~' x, X = ---- = ---- (7) (8) (9) Page 8 Titles 108 x; _ t.; Ii~' RI Rp,e (10) Xa Xp etc . X. + Xa + Xp + ... = 1, Page 9 Titles 109 (13) Page 10 Titles 110 (14) (Gik)2__l_. (15) Ire' A, is (%A)mixture = (%A)IXI + (%A)2X2 + ... + (%A)kXk + E, (17) Page 11 Titles 111 Page 12 Titles 112 Page 13 Titles 113 Tables Table 1 Page 14 Titles 114 NBK POINTS NBK POINTS (OPTIONAL) NBK POINTS NBK POINTS ­ Page 7 Titles 255 Page 8 Titles 256 o o :2 o o :2 Page 9 Titles 257 Page 10 Titles SiN 10. Single. Constrained. SiN 10. Single. Unconstrained. wi Noise Alpha-stripped. WI Noise Alpha-stripped. wiD Noise o Tables Table 1 Table 2 Page 11 Titles 259 Page 12 Titles 260 a :2 300 iii I 300 Iii i I Tables Table 1 Page 13 Titles 261 Page 14 Titles 262 Page 15 Titles 263 Tan e E • m front. FWHM front :=:;:;;:HM bock ! It' Two-theta Page 16 Titles 264 Page 17 Tables Table 1 Page 18 Titles 266 Page 19 Titles 267 exp[ -(f3clf3g)2 11' 1 1 - erf[ (1/11' il2 (/3clf3g) 1 /3c /3 l f3g 12 ------ I /3 J l r J1I' /3/ 1 1 L /3 /3i 11' J J Page 20 Titles 268 Page 21 Titles 47 48 Two-Theta 49 269 Tables Table 1 Page 22 Titles 270 Page 23 Titles 271 SUMMARY Page 24 Titles 272 Page 25 Titles 273 Page 26 Titles 274 Page 27 Titles 275 Page 28 Page 1 Titles 9. RIETVELD REFINEMENT OF CRYSTAL STRUCTURES J.E. Post & D.L. Bish Page 2 Tables Table 1 Page 3 Titles 279 Page 4 Titles 280 Page 5 Titles 281 Page 6 Titles 282 Page 7 Titles 283 Page 8 Titles 284 (5) Page 9 Titles '0 Tables Table 1 Page 10 Titles 286 Page 11 Titles 287 Page 12 Titles 288 ~ Page 13 Titles 289 Page 14 Titles 290 Page 15 Titles 291 ~ ~ Page 16 Titles 292 Page 17 Titles 293 Page 18 Titles 294 Page 19 Titles 295 Page 20 Titles 296 Page 21 Titles 297 Page 22 Titles 298 .~.1!. .9:~.~? _. ._.9:9.~? _9:9.~? __ ._ Tables Table 1 Page 23 Tables Table 1 Page 24 Titles 300 Page 25 Titles 301 Page 26 Titles 302 '~~-ato~~siti:~~s-fui~'F~;;ri~'diii~~~;';~~';;;ap---"''''------- -.---- - - .. ------- Cs Clinoptilolite A. B. Page 27 Titles o. b. ... Todorokite. #126232, South Africa Theta (Degrees) Tables Table 1 Page 28 Titles 304 Page 29 Titles 305 Page 30 Titles 306 Page 31 Titles 307 Page 32 Titles 308 Page 1 Titles 10. SYNCHROTRON POWDER DIFFRACTION L.W. Finger Page 2 Titles 310 ~ .,. &.~Jr; " "'""v Page 3 Page 4 Titles 312 Page 5 Titles 313 -- - --- __ ~« I - Page 6 Page 7 Titles 315 SP m 00 ~ W 00 m 00 00 m 10 o Page 8 Titles 316 Page 9 Page 10 Page 11 Titles 319 >­ 01 . nI.......... ....... .. _ .. t' I (a) ~ E I (b) 67.5 68.0 Page 12 Titles 320 Page 13 Page 14 Titles 322 10 20 30 15.0 15.1 15.2 Tables Table 1 Page 15 Page 16 Page 17 Titles 325 3000 2000 1000 a 17 20 23 26 Tables Table 1 Table 2 Page 18 Titles 326 Page 19 Page 20 Titles 328 1.0 0.5 0.0 o 20 40 60 80 Energy, keY o 1 µt 2 3 Page 21 Page 22 Titles 330 Page 23 Titles 331 Page 24 Page 1 Titles 11. NEUTRON POWDER DIFFRACTION R.B. Von Dreele Page 2 Titles 334 Tables Table 1 Page 3 Titles 335 A =l!_ Page 4 Titles 336 Page 5 Titles " , " , , , , " : ' I' I II : : ,,r: , s ------------------ S = S - So = h 337 sin eo. Tables Table 1 Page 6 Titles 338 Page 7 Tables Table 1 Page 8 Titles 340 1 E 1 00 u Tables Table 1 Table 2 Table 3 Page 9 Page 10 Titles 342 FWHM 0-2" o·{ o· 0 50 , ~/ , 0.4 0.8 1.0 1 .2 1.4 Page 11 Titles 343 A)2 2 Page 12 Titles 344 ~~~' - , -~ ot30"''" LAMPF PSR WNR Page 13 Titles 345 h ' (21) Page 14 Titles 346 o 7.0 5.0 1.0 2.0 y----to-to--t~~~=t= Tables Table 1 Page 15 Titles 347 Page 16 Titles 348 GENERAL PURPOSE DIFFRACTOMETER 4.0 5,0 6.0 8. Tables Table 1 Page 17 Titles 349 I ~ '" 8 o Tables Table 1 Table 2 Page 18 Titles 350 Page 19 Titles 351 TOP, µsec Page 20 Titles 352 1'0 (28) (29) (30) (31) (32) (33) (34) T'n = I,CmXm (35) X=(2/T)-1 (36) Page 21 Titles 353 Page 22 Titles 354 Page 23 Titles 355 v = ~130"2 - MT) (130"2 - .1 T) Page 24 Titles 356 M M Tables Table 1 Page 25 Titles 357 Ad Page 26 Titles 358 fA p x M Page 27 Titles 359 X =M Page 28 Titles 360 Tables Table 1 Page 29 Titles 361 Page 30 Titles 362 Page 31 Titles 363 Page 32 Titles 364 Tables Table 1 Page 33 Tables Table 1 Page 34 Titles 366 Page 35 Titles 367 Page 36 Titles 368 Page 37 Titles 369 Page 38