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227 | |
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228 | <h1>Stacking Fault Simulations II</h1> |
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229 | |
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230 | <p class=MsoNormal>In this exercise and the next you will simulate some |
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231 | diffraction patterns from kaolinite clays. Kaolinite, Al<sub>2</sub>Si<sub>2</sub>O<sub>5</sub>(OH)<sub>4</sub>, |
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232 | is a 1:1 layer silicate with a single unique sheet with AlO<sub>6</sub> |
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233 | octahedra on one side and SiO<sub>4</sub> tetrahedra on the other. The layers |
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234 | stack with an offset to ideally form a triclinic C1 lattice (Bish & Von |
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235 | Dreele, 1989, Clay & Clay Min. 37, 289-296) for a sample of the most |
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236 | ordered form of kaolinite from Keokuk, Iowa. Kaolinites from other locations |
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237 | evidently have stacking faults so that the peaks are displaced, have peculiar |
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238 | shapes and are above a varying background. For the exercise we provide a |
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239 | laboratory Bragg-Brentano pattern of Keokuk kaolinite collected with CuKa |
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240 | radiation on a Bruker instrument and thus in the Bruker RAW file format. The |
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241 | Keokuk kaolinite has some dickite (different ordered stacking of kaolinite |
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242 | layers). The next exercise Stacking Faults-III) covers a simple simulation of a |
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243 | faulted kaolinite from Georgia.</p> |
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244 | |
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245 | <p class=MsoNormal>If you have not done so already, start GSAS-II.</p> |
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246 | |
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247 | <h2>Part 1. Creating kaolinite layer</h2> |
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248 | |
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249 | <p class=MsoNormal>In this initial step we will load from a cif file the |
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250 | structure of kaolinite, draw it to see the layer structure and then transform |
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251 | it into forms suitable for stacking simulations. To begin do <b><span |
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252 | style='font-family:"Calibri",sans-serif'>Import/Phase/from CIF file</span></b>; |
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253 | from the file dialog select <b><span style='font-family:"Calibri",sans-serif'>kaolinite.cif</span></b>. |
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254 | After the are you sure popup, there will be another warning you that 4 atom |
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255 | types (O-H) were not recognized chemical element symbols and they were |
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256 | substituted by Xe to make them obvious in the atom list. Press <b><span |
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257 | style='font-family:"Calibri",sans-serif'>Ok</span></b>; you are offered a |
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258 | chance to change the phase name, I used <b><span style='font-family:"Calibri",sans-serif'>kaolinite</span></b>. |
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259 | The General tab is displayed (notice the presence of Xe in the element table).</p> |
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260 | |
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261 | <p class=MsoNormal><img width=930 height=500 |
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262 | src="Stacking%20Faults%20II_files/image001.gif"></p> |
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263 | |
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264 | <p class=MsoNormal>To fix the Xe atoms (they should be O), select <b><span |
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265 | style='font-family:"Calibri",sans-serif'>Atoms</span></b> and then double click |
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266 | the <b><span style='font-family:"Calibri",sans-serif'>Type</span></b> column |
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267 | heading; a small popup will appear. Select <b><span style='font-family:"Calibri",sans-serif'>Xe</span></b> |
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268 | & press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>; |
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269 | the Xe atoms at the bottom of the atom table will be highlighted. Next select <b><span |
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270 | style='font-family:"Calibri",sans-serif'>Edit/Modify atom parameters</span></b> |
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271 | from the Phase Data menu; a new popup will appear. Select <b><span |
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272 | style='font-family:"Calibri",sans-serif'>Type</span></b> & press <b><span |
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273 | style='font-family:"Calibri",sans-serif'>Ok</span></b>; a periodic table of the |
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274 | element will appear. Select <b><span style='font-family:"Calibri",sans-serif'>O</span></b> |
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275 | from the O-atom pulldown; the structure will be drawn with Al, Si & O atoms |
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276 | only.</p> |
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277 | |
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278 | <p class=MsoNormal><img width=479 height=358 |
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279 | src="Stacking%20Faults%20II_files/image003.jpg"></p> |
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280 | |
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281 | <p class=MsoNormal>To better visualize the stacking layer, select the <b><span |
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282 | style='font-family:"Calibri",sans-serif'>Draw Atoms</span></b> tab and then |
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283 | double click the empty upper left corner box of the table. All atoms will turn |
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284 | green. Then do <b><span style='font-family:"Calibri",sans-serif'>Edit/Fill unit |
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285 | cell</span></b>; the structure will be redrawn with all atoms that belong in |
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286 | the unit cell. Finally, double click on the <b><span style='font-family:"Calibri",sans-serif'>Type</span></b> |
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287 | column heading, select <b><span style='font-family:"Calibri",sans-serif'>Al</span></b> |
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288 | & <b><span style='font-family:"Calibri",sans-serif'>Si</span></b> (they |
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289 | will turn green) and then do <b><span style='font-family:"Calibri",sans-serif'>Edit/Fill |
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290 | CN sphere</span></b>. After a bit of rotating the structure around, the |
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291 | layering along the c-axis (blue line) will be evident.</p> |
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292 | |
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293 | <p class=MsoNormal><img width=480 height=359 |
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294 | src="Stacking%20Faults%20II_files/image004.jpg"></p> |
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295 | |
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296 | <p class=MsoNormal>One can easily see the layer of SiO<sub>4</sub> tetrahedra |
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297 | and AlO<sub>6</sub> octahedra. Also notice that the next layer (represented by |
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298 | the 4 O atoms at the bottom of the above drawing are offset giving a triclinic |
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299 | lattice.</p> |
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300 | |
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301 | <p class=MsoNormal>The stacking fault simulation calculation via DIFFaX |
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302 | routines requires that the stacking layers be defined in a coordinate system |
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303 | that has the stacking direction perpendicular to the stacking plane defined as |
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304 | the c-axis. This requires transformation of the unit cell and atom coordinates; |
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305 | a suitable tool exists in GSAS-II to do this. Select the <b><span |
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306 | style='font-family:"Calibri",sans-serif'>General</span></b> tab and do <b><span |
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307 | style='font-family:"Calibri",sans-serif'>Compute/Transform</span></b>; a popup |
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308 | window will appear.</p> |
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309 | |
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310 | <p class=MsoNormal><img width=350 height=339 |
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311 | src="Stacking%20Faults%20II_files/image005.gif"></p> |
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312 | |
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313 | <p class=MsoNormal>Note that this allows one to transform the structure |
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314 | according to a matrix and then shift the resultant positions along some vector |
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315 | and then select those that are unique according to a selected space group. The |
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316 | pulldown gives a selection of commonly used transformations; we want the last |
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317 | one, <b><span style='font-family:"Calibri",sans-serif'>abc*</span></b>, which |
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318 | satisfies the stacking fault requirement. Select it; notice that the space |
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319 | group is changed to P1. Leave this as the kaolinite layer has no symmetry; in |
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320 | other circumstances the layer may have an inversion center in which case P-1 |
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321 | should be used. If you press <b><span style='font-family:"Calibri",sans-serif'>Test</span></b>, |
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322 | the new lattice parameters will be shown.</p> |
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323 | |
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324 | <p class=MsoNormal><img width=350 height=339 |
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325 | src="Stacking%20Faults%20II_files/image006.gif"></p> |
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326 | |
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327 | <p class=MsoNormal>The a & b axes stay the same, but c is now smaller (the |
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328 | interlayer distance in kaolinite) and <span style='font-family:Symbol'>a</span> |
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329 | & <span style='font-family:Symbol'>b</span> = 90 (<span style='font-family: |
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330 | Symbol'>g</span> is unchanged). Press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>; |
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331 | a new phase (kaolinite abc*) will be made and its General tab will be shown |
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332 | immediately. Select the <b><span style='font-family:"Calibri",sans-serif'>Draw |
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333 | Atoms</span></b> tab to see the resulting structure.</p> |
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334 | |
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335 | <p class=MsoNormal><img width=471 height=352 |
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336 | src="Stacking%20Faults%20II_files/image007.jpg"></p> |
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337 | |
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338 | <p class=MsoNormal>To see what this layer looks like with more of it drawn, you |
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339 | can add more unit cells to the drawing; select all the atoms by double clicking |
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340 | the upper left empty box of the Draw atoms table. Do <b><span style='font-family: |
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341 | "Calibri",sans-serif'>Edit/Add atoms</span></b> and <b><span style='font-family: |
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342 | "Calibri",sans-serif'>increment</span></b> the 1<sup>st</sup> <b><span |
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343 | style='font-family:"Calibri",sans-serif'>Choose unit cel</span></b>l and press <b><span |
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344 | style='font-family:"Calibri",sans-serif'>Ok</span></b>; this will add one unit |
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345 | cell along x. Now select all the atoms again, do <b><span style='font-family: |
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346 | "Calibri",sans-serif'>Edit/Add atoms</span></b> and now <b><span |
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347 | style='font-family:"Calibri",sans-serif'>decrement</span></b> the 1<sup>st</sup> |
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348 | <b><span style='font-family:"Calibri",sans-serif'>Choose unit cell</span></b>. |
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349 | Press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>; the |
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350 | drawing will now be 3 unit cells wide along x. Repeat this once more <b><span |
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351 | style='font-family:"Calibri",sans-serif'>decrementing</span></b> the 2<sup>nd</sup> |
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352 | <b><span style='font-family:"Calibri",sans-serif'>Choose unit cell</span></b> |
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353 | to give a 3x2 unit cell block of atoms. Double click the <b><span |
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354 | style='font-family:"Calibri",sans-serif'>Style</span></b> column heading and |
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355 | select <b><span style='font-family:"Calibri",sans-serif'>Balls and sticks</span></b>; |
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356 | the drawing should look like (after some zooming/shifting/rotation).</p> |
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357 | |
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358 | <p class=MsoNormal><img width=477 height=357 |
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359 | src="Stacking%20Faults%20II_files/image009.jpg"></p> |
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360 | |
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361 | <p class=MsoNormal>This structure is now suitable for use in DIFFaX |
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362 | calculations; the cell has a c-axis that is perpendicular to the ab plane with |
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363 | a length that is the stacking repeat distance. This is a good place to save |
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364 | your project (I called it <b><span style='font-family:"Calibri",sans-serif'>kaolinite</span></b>).</p> |
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365 | |
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366 | <h2>Part 2. Set up simulation of ideal kaolinite stacking</h2> |
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367 | |
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368 | <p class=MsoNormal>In this part of the tutorial well create a stacking model |
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369 | for Keokuk kaolinite and use DIFFaX to simulate the powder pattern and compare |
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370 | it to some real data. To begin we need a new phase that we can declare as |
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371 | faulted. In the main GSAS-II data tree menu do <b><span style='font-family: |
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372 | "Calibri",sans-serif'>Data/Add new phase</span></b>; I named it <b><span |
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373 | style='font-family:"Calibri",sans-serif'>Keokuk</span></b>. The General tab |
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374 | for it will immediately appear.</p> |
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375 | |
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376 | <p class=MsoNormal><img width=930 height=500 |
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377 | src="Stacking%20Faults%20II_files/image010.gif"></p> |
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378 | |
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379 | <p class=MsoNormal>Change the <b><span style='font-family:"Calibri",sans-serif'>Phase |
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380 | type</span></b> to <b><span style='font-family:"Calibri",sans-serif'>faulted</span></b>; |
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381 | the General tab will be redrawn and a new tab <b><span style='font-family:"Calibri",sans-serif'>Layers</span></b> |
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382 | will appear. Select it.</p> |
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383 | |
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384 | <p class=MsoNormal><img width=817 height=484 |
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385 | src="Stacking%20Faults%20II_files/image011.gif"></p> |
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386 | |
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387 | <p class=MsoNormal>We can anticipate (given that kaolinite space group is C1) |
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388 | that the <b><span style='font-family:"Calibri",sans-serif'>Diffraction Laue |
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389 | symmetry</span></b> is <b><span style='font-family:"Calibri",sans-serif'>-1</span></b>. |
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390 | We can enter by hand the lattice parameters from the kaolinite abc* phase but |
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391 | an easier method is available. Do <b><span style='font-family:"Calibri",sans-serif'>Operations/Copy |
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392 | phase cell</span></b>; a file selection dialog will appear for your current |
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393 | directory and the file <b><span style='font-family:"Calibri",sans-serif'>kaolinite.gpx</span></b> |
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394 | should be there. Select it; a small popup will appear listing the available |
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395 | phases. Choose <b><span style='font-family:"Calibri",sans-serif'>kaolinite |
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396 | abc*</span></b> and press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>; |
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397 | the Layers window will be redrawn with the new lattice parameters.</p> |
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398 | |
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399 | <p class=MsoNormal><img width=829 height=484 |
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400 | src="Stacking%20Faults%20II_files/image012.gif"></p> |
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401 | |
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402 | <p class=MsoNormal>Next, you need to define the layer. As it would be very |
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403 | tedious to enter 24 atoms by hand, the alternative is to get them from the |
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404 | previously created kaolinite abc* phase. Select the <b><span style='font-family: |
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405 | "Calibri",sans-serif'>Import new layer</span></b> box; the file dialog with <b><span |
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406 | style='font-family:"Calibri",sans-serif'>kaolinite.gpx</span></b> will appear. |
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407 | Select the file and press <b><span style='font-family:"Calibri",sans-serif'>Open</span></b>; |
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408 | again a small popup with two phases listed will appear. Again select <b><span |
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409 | style='font-family:"Calibri",sans-serif'>kaolinite abc*</span></b> and press <b><span |
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410 | style='font-family:"Calibri",sans-serif'>Ok</span></b>; the Layers page will be |
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411 | redrawn with a layer (named kaolinite) will be filled out.</p> |
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412 | |
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413 | <p class=MsoNormal><img width=829 height=500 |
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414 | src="Stacking%20Faults%20II_files/image013.gif"></p> |
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415 | |
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416 | <p class=MsoNormal>If you move down to the bottom of the page (if there isnt a |
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417 | scroll bar, just grab an edge of the window & shift it slightly) to find |
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418 | the one line <b><span style='font-family:"Calibri",sans-serif'>Layer-Layer |
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419 | Transition probabilities</span></b>. Change <b><span style='font-family:"Calibri",sans-serif'>Dz=1.0</span></b> |
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420 | and press the plot box; the drawing will show a layer of kaolinite stacked |
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421 | directly above another one.</p> |
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422 | |
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423 | <p class=MsoNormal><img width=480 height=359 |
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424 | src="Stacking%20Faults%20II_files/image014.jpg"></p> |
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425 | |
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426 | <p class=MsoNormal>Compare that to the stacking in kaolinite.</p> |
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427 | |
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428 | <p class=MsoNormal><img width=480 height=359 |
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429 | src="Stacking%20Faults%20II_files/image015.jpg"></p> |
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430 | |
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431 | <p class=MsoNormal>Notice the effect of the offset. The 1<sup>st</sup> row of |
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432 | SiO<sub>4</sub> tetrahedra are positioned directly above the AlO<sub>6</sub> |
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433 | octahedra in the real structure but not in the vertically stacked structure. We |
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434 | can use a bit of simple geometry to work out what the offset is but first let |
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435 | us see what happens in the simulation and how it compares to real data.</p> |
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436 | |
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437 | <h2>Step 3. Import Keokuk kaolinite data and do 1<sup>st</sup> simulation</h2> |
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438 | |
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439 | <p class=MsoNormal>First we need to import the Keokuk kaolinite powder data; do |
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440 | <b><span style='font-family:"Calibri",sans-serif'>Import/Powder Data/from |
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441 | Bruker RAW file</span></b>. Select <b><span style='font-family:"Calibri",sans-serif'>Keokuk |
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442 | kaolinite.RAW</span></b> from the file dialog box; press <b><span |
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443 | style='font-family:"Calibri",sans-serif'>Yes</span></b> in the next popup. A |
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444 | new file dialog appears requesting an instrument parameter file; we will use an |
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445 | internal default instead. Press <b><span style='font-family:"Calibri",sans-serif'>Cancel</span></b> |
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446 | and select <b><span style='font-family:"Calibri",sans-serif'>Defaults for CuKa |
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447 | lab data</span></b> from the next popup. This process will repeat since the RAW |
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448 | file contains two scans. In the next popup, select only <b><span |
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449 | style='font-family:"Calibri",sans-serif'>kaolinite abc*</span></b>. There will |
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450 | be two PWDR scans in the GSAS-II data tree; one covers 2<span style='font-family: |
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451 | Symbol'>Q</span>= 10-90<span style='font-family:"Calibri",sans-serif'>°</span> |
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452 | and the other covers 2<span style='font-family:Symbol'>Q</span>=80-150°. Only |
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453 | the lower part of the first one is going to be used in our simulation work as the |
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454 | calculations become very time consuming for complex structures and high angle |
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455 | data. Select <b><span style='font-family:"Calibri",sans-serif'>PWDR Keokuk |
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456 | kaolinite.RAW Scan 1</span></b> from the GSAS-II data tree make sure it |
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457 | expands; its plot will also show.</p> |
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458 | |
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459 | <p class=MsoNormal><img width=700 height=600 |
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460 | src="Stacking%20Faults%20II_files/image016.gif"></p> |
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461 | |
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462 | <p class=MsoNormal>Go to <b><span style='font-family:"Calibri",sans-serif'>Limits</span></b> |
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463 | and set <b><span style='font-family:"Calibri",sans-serif'>Tmax</span></b> to <b><span |
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464 | style='font-family:"Calibri",sans-serif'>52.0</span></b>; that puts the upper limit |
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465 | in a relatively clear part of the pattern. Then go to Background and set the 1<sup>st</sup> |
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466 | coefficient to 20 (approximately the background at 2Q=18). Next go to <b><span |
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467 | style='font-family:"Calibri",sans-serif'>Sample parameters</span></b> and set |
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468 | the <b><span style='font-family:"Calibri",sans-serif'>Histogram scale</span></b> |
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469 | to something reasonable (I chose <b><span style='font-family:"Calibri",sans-serif'>20.0</span></b>) |
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470 | and make sure the <b><span style='font-family:"Calibri",sans-serif'>Diffractometer |
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471 | type is Bragg-Brentano</span></b>.</p> |
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472 | |
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473 | <p class=MsoNormal>Now we are ready for our 1<sup>st</sup> kaolinite |
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474 | simulation. Go to <b><span style='font-family:"Calibri",sans-serif'>Phases/Keokuk</span></b> |
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475 | and select the <b><span style='font-family:"Calibri",sans-serif'>Layers</span></b> |
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476 | tab. Do <b><span style='font-family:"Calibri",sans-serif'>Operations/Simulate |
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477 | pattern</span></b> and press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b> |
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478 | in the popup. Select the <b><span style='font-family:"Calibri",sans-serif'>Scan |
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479 | 1</span></b> pattern and press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>; |
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480 | the simulation will finish quickly (press <b><span style='font-family:"Calibri",sans-serif'>Ok</span></b>) |
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481 | and the new plot will be displayed (Ive zoomed in a bit).</p> |
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482 | |
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483 | <p class=MsoNormal><img width=700 height=600 |
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484 | src="Stacking%20Faults%20II_files/image017.gif">.</p> |
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485 | |
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486 | <p class=MsoNormal>As you can see the simulation (green curve) does not fit the |
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487 | data (blue crosses) at all mostly due to the incorrect layer offset although |
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488 | the 1<sup>st</sup> peak seems to be positioned correctly. To work out the |
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489 | offset consider the drawing of kaolinite.</p> |
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490 | |
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491 | <p class=MsoNormal><img width=480 height=338 |
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492 | src="Stacking%20Faults%20II_files/image002.gif"></p> |
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493 | |
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494 | <p class=MsoNormal>The offset Dx is given by the blue arrow in the above |
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495 | drawing of kaolinite and is in fractional coordinates. Geometry gives</p> |
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496 | |
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497 | <p class=MsoNormal><span style='position:relative;top:3pt'><img width=106 |
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498 | height=26 src="Stacking%20Faults%20II_files/image021.gif"> Or in this case |
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499 | <b><span style='font-family:"Calibri",sans-serif'>-0.368</span></b>. Set <b><span |
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500 | style='font-family:"Calibri",sans-serif'>Dx</span></b> to this value & |
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501 | repeat simulation.</p> |
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502 | |
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503 | <p class=MsoNormal><img width=700 height=600 |
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504 | src="Stacking%20Faults%20II_files/image022.gif"></p> |
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505 | |
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506 | <p class=MsoNormal>There is some improvement but some parts are not very well |
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507 | represented. Recall from the triclinic kaolinite lattice parameters that <span |
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508 | style='font-family:Symbol'>a</span> was 91.7°; that will produce a small offset |
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509 | in Dy. Using the same kind of geometry math gives <b><span style='font-family: |
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510 | "Calibri",sans-serif'>Dy=-0.0246</span></b>. Enter this value & repeat the |
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511 | simulation again. This gives a much better fit to the observed pattern, but the |
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512 | simulated peaks are too sharp; this can be fixed by changing the U,V,W |
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513 | Instrument parameters. Id just set <b><span style='font-family:"Calibri",sans-serif'>W=40</span></b> |
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514 | and the <b><span style='font-family:"Calibri",sans-serif'>Histogram scale</span></b> |
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515 | (in <b><span style='font-family:"Calibri",sans-serif'>Sample parameters</span></b>) |
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516 | to <b><span style='font-family:"Calibri",sans-serif'>40</span></b> and try |
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517 | again.</p> |
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518 | |
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519 | <p class=MsoNormal><img width=700 height=600 |
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520 | src="Stacking%20Faults%20II_files/image023.gif"></p> |
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521 | |
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522 | <p class=MsoNormal>That is a pretty good fit for a stacking simulation. By |
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523 | further hand tweaking of the parameters one can further improve the simulation |
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524 | but based on what we see here we do have the right description of stacking in |
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525 | Keokuk kaolinite. Doing sequence simulations varying each parameter over a |
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526 | small range can be used to help with optimization, but in this case it would be |
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527 | far easier to do a Rietveld refinement for this well ordered kaolinite. Save |
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528 | your project as you will need it for the next exercise (Stacking Faults-III).</p> |
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529 | |
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530 | </span></div> |
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531 | |
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532 | </body> |
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533 | |
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534 | </html> |
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