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chanerwang木蟲 (著名寫手)
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[求助]
求助XRD精修，請(qǐng)問(wèn)如何通過(guò)精修看出摻雜的元素進(jìn)入到晶格中，和產(chǎn)生更多的氧空位？
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審稿專家的評(píng)語(yǔ)：In fact it is contradictory because using XPS authors detected the presence of europium on BiVO4 surface, then why authors assume that it is into the crystal structure of compound. Also cell volume is lower when sample contains boron and europium than sample BiVO4, normally when some cation, boron or europium, is incorporated into the lattice volume tends to increase. On the other hand, authors mentioned that samples contained high amount of surface oxygen vacancies, I would like to mention that by using XRD Rietveld analysis it is possible to determine the oxygen vacancies in samples, it is better if authors try to corroborate such affirmation doing XRD Rietveld analysis. Additionally, through XRD Rietveld method authors can obtain the cell parameters of all samples and compare them in order to corroborate if boron and europium are into the crystal structure, just the crystal size and volume value are not enough evidence. 我完全不太會(huì)用這個(gè)，求助啊，我該如何做呢？好不容易審稿回來(lái)的意見(jiàn)，不敢不重視啊  |
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lqingh506
鐵桿木蟲 (知名作家)
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10樓2013-08-26 06:53:12
lqingh506
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【答案】應(yīng)助回帖
★ ★ ★ ★ ★
感謝參與，應(yīng)助指數(shù) +1
chanerwang: 金幣+5, ★★★很有幫助 2013-07-05 22:12:42
感謝參與，應(yīng)助指數(shù) +1
chanerwang: 金幣+5, ★★★很有幫助 2013-07-05 22:12:42
| 審稿人是要你對(duì)硼和銪摻雜后樣品的XRD做Rietveld精修，從而獲得更精確的晶胞參數(shù)，再通過(guò)氧原子的占位率判斷是否存在氧缺陷。你可能需要收集精度更高的XRD數(shù)據(jù)，再采用GSAS、MS、Fullprof、Manud等軟件對(duì)XRD做Rietveld精修，僅供樓主參考，希望對(duì)你有幫助，祝好！ |
chanerwang2樓2013-07-05 21:25:04
chanerwang
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3樓2013-07-05 22:12:27
lqingh506
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4樓2013-07-06 08:17:20
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5樓2013-07-06 09:24:32
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6樓2013-07-06 09:44:25
chanerwang
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我也不知道，就是在表征的時(shí)候讓表征的老師幫忙算了下，有一個(gè)text文件。你能幫看看嗎？ USER: Administrator JADE: Cell Refinement Report DATE: Sunday, May 06, 2012 08:24p FILE: [WM-6110.DAT] SCAN: 10.02/79.9783/0.02/1(sec), Cu, I(max)=10973, 05/06/12 18:45 PEAK: 23-pts/Parabolic Filter, Threshold=3.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Summit NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54056? (Cu/K-alpha1) Cell Type = Monoclinic, I2/b (15) <c-unique> Initial Cell = 5.1935 x 5.0898 x 11.6972 <90.0 x 90.0 x 90.387> Refined Cell = 5.18863(0.010795), 5.09036(0.009739), 11.69668(0.000228) [90.2856(0.00618)] Vol= 308.93 A^3, Density(c)= 6.9640 (Chemical Formula =BiVO4, Z=4.0) Two-Theta Error Window = 0.3(deg), Zero Offset = 0.0(deg), Displacement = 0.0(deg) ESD of Fit = 0.0366(deg), |Delta 2-Theta| = 0.0265(deg), |Delta d| = 0.00111(?), F(30) = 20.8(61) Intensity Weighting = Sqrt(I%), Two-Theta Range = 10.02/79.98(deg), (x) Outlier Rejection at 2.0 sigmas 2T(cor) = 2T(obs) - Zero Offset - Displacement (cal=Calculated, obs=Observed, cor=Corrected) ( h k l) 2T(cal) 2T(cor) 2T(obs) Delta d(cal) d(cor) d(obs) Del-d ? ( 0 0 2) 15.137 15.141 15.141 -0.005 5.8483 5.8466 5.8466 0.0018 ( 1 0 1) 18.693 --- 4.7429 --- ( 0 1 1) 18.998 18.979 18.979 0.020 4.6675 4.6722 4.6722 -0.0048 ( 1 0 3) 28.615 --- 3.1170 --- ( 0 1 3) 28.820 28.880 28.880 -0.060 3.0953 3.0890 3.0890 0.0063 ( 1 1 2) 28.957 --- 3.0809 --- ( 0 0 4) 30.546 30.539 30.539 0.007 2.9242 2.9248 2.9248 -0.0006 ( 2 0 0) 34.545 34.540 34.540 0.004 2.5943 2.5946 2.5946 -0.0003 ( 0 2 0) 35.233 35.198 35.198 0.035 2.5451 2.5476 2.5476 -0.0025 ( 2 0 2) 37.909 37.879 37.879 0.030 2.3714 2.3732 2.3732 -0.0018 ( 0 2 2) 38.545 --- 2.3337 --- (-1 1 4) 39.485 39.519 39.519 -0.034 2.2803 2.2785 2.2785 0.0019 ( 1 1 4) 39.565 --- 2.2759 --- ( 2 1 1) 39.797 39.858 39.858 -0.061 2.2632 2.2599 2.2599 0.0033 (-1 2 1) 40.097 40.039 40.039 0.059 2.2469 2.2501 2.2501 -0.0032 ( 1 2 1) 40.256 40.235 40.235 0.021 2.2384 2.2395 2.2395 -0.0011 ( 1 0 5) 42.347 --- 2.1326 --- ( 0 1 5) 42.493 42.460 42.460 0.032 2.1256 2.1272 2.1272 -0.0016 (-2 1 3) 45.515 45.478 45.478 0.037 1.9912 1.9928 1.9928 -0.0015 ( 2 1 3) 45.659 45.604 45.604 0.055 1.9853 1.9876 1.9876 -0.0023 (-1 2 3) 45.928 45.958 45.958 -0.030 1.9743 1.9731 1.9731 0.0012 ( 1 2 3) 46.070 46.097 46.097 -0.027 1.9685 1.9674 1.9674 0.0011 ( 0 0 6) 46.548 --- 1.9494 --- ( 2 0 4) 46.772 46.760 46.760 0.012 1.9406 1.9411 1.9411 -0.0005 ( 0 2 4) 47.310 47.299 47.299 0.011 1.9198 1.9202 1.9202 -0.0004 (-2 2 0) 50.038 50.018 50.018 0.020 1.8214 1.8220 1.8220 -0.0007 ( 2 2 0) 50.305 50.299 50.299 0.006 1.8123 1.8125 1.8125 -0.0002 (-2 2 2) 52.585 52.639 52.639 -0.054 1.7390 1.7373 1.7373 0.0017 ( 2 2 2) 52.842 --- 1.7311 --- (-1 1 6) 53.250 53.260 53.260 -0.009 1.7188 1.7185 1.7185 0.0003 ( 1 1 6) 53.314 --- 1.7169 --- ( 3 0 1) 53.515 --- 1.7109 --- ( 0 3 1) 54.609 54.621 54.621 -0.012 1.6792 1.6789 1.6789 0.0003 (-2 1 5) 55.810 --- 1.6459 --- ( 2 1 5) 55.934 55.859 55.859 0.075 1.6425 1.6446 1.6446 -0.0020 x (-1 2 5) 56.166 --- 1.6363 --- ( 1 2 5) 56.290 --- 1.6330 --- ( 1 0 7) 57.933 57.919 57.919 0.014 1.5905 1.5909 1.5909 -0.0003 ( 0 1 7) 58.049 --- 1.5876 --- ( 3 0 3) 58.317 --- 1.5810 --- ( 3 1 2) 58.570 58.438 58.438 0.132 1.5747 1.5780 1.5780 -0.0032 x ( 2 0 6) 59.241 59.239 59.239 0.002 1.5585 1.5585 1.5585 0.0000 ( 1 3 2) 59.489 --- 1.5526 --- ( 0 2 6) 59.698 --- 1.5476 --- ( 2 2 4) 60.005 59.999 59.999 0.006 1.5404 1.5406 1.5406 -0.0001 ( 0 0 8) 63.584 63.580 63.580 0.004 1.4621 1.4622 1.4622 -0.0001 (-3 1 4) 65.162 64.879 64.879 0.283 1.4304 1.4360 1.4360 -0.0056 x ( 3 1 4) 65.331 65.337 65.337 -0.005 1.4271 1.4270 1.4270 0.0001 (-3 2 1) 65.537 --- 1.4232 --- ( 3 2 1) 65.874 --- 1.4167 --- (-1 3 4) 66.027 66.018 66.018 0.009 1.4138 1.4140 1.4140 -0.0002 ( 1 3 4) 66.195 --- 1.4106 --- ( 2 3 1) 66.413 66.441 66.441 -0.029 1.4065 1.4060 1.4060 0.0005 ( 3 0 5) 67.266 67.257 67.257 0.009 1.3907 1.3909 1.3909 -0.0002 ( 0 3 5) 68.224 68.138 68.138 0.086 1.3735 1.3750 1.3750 -0.0015 x ( 1 1 8) 69.233 69.219 69.219 0.015 1.3559 1.3562 1.3562 -0.0003 ( 2 1 7) 69.391 --- 1.3532 --- (-1 2 7) 69.597 --- 1.3497 --- ( 1 2 7) 69.707 69.759 69.759 -0.052 1.3479 1.3470 1.3470 0.0009 ( 3 2 3) 70.163 70.161 70.161 0.002 1.3402 1.3403 1.3403 0.0000 (-2 3 3) 70.359 --- 1.3370 --- (-2 2 6) 70.729 70.561 70.561 0.168 1.3309 1.3336 1.3336 -0.0028 x ( 2 2 6) 70.946 70.979 70.979 -0.033 1.3273 1.3268 1.3268 0.0005 ( 4 0 0) 72.858 72.838 72.838 0.020 1.2971 1.2975 1.2975 -0.0003 ( 2 0 8) 74.421 74.400 74.400 0.021 1.2737 1.2740 1.2740 -0.0003 ( 0 4 0) 74.500 --- 1.2726 --- ( 0 2 8) 74.829 74.760 74.760 0.069 1.2678 1.2688 1.2688 -0.0010 ( 0 1 9) 75.426 --- 1.2592 --- (-3 1 6) 75.725 --- 1.2550 --- ( 3 1 6) 75.883 75.957 75.957 -0.074 1.2528 1.2517 1.2517 0.0010 x (-1 3 6) 76.536 76.599 76.599 -0.063 1.2437 1.2428 1.2428 0.0009 ( 1 3 6) 76.694 --- 1.2415 --- (-1 4 1) 77.509 --- 1.2305 --- ( 1 4 1) 77.719 77.653 77.653 0.066 1.2277 1.2286 1.2286 -0.0009 (-3 2 5) 78.115 --- 1.2225 --- ( 3 2 5) 78.430 78.397 78.397 0.033 1.2184 1.2188 1.2188 -0.0004 (-2 3 5) 78.618 78.637 78.637 -0.019 1.2159 1.2157 1.2157 0.0002 ( 2 3 5) 78.932 79.059 79.059 -0.128 1.2119 1.2102 1.2102 0.0016 x ( 3 0 7) 79.730 --- 1.2017 --- (-4 1 3) 80.057 --- 1.1976 --- |
7樓2013-07-06 09:55:25
綠色西工
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8樓2013-07-12 11:29:00
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9樓2013-08-25 19:47:04
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