X射線衍射實驗報告(共11頁)

1、中 南 大 學(xué)X射線衍射實驗報告材料科學(xué)與工程學(xué)院材料國際專業(yè)1401班級姓 名蔡云偉學(xué)號0605140118同組者 實驗日期2016年05月18日指導(dǎo)教師黃繼武評分分評閱人評閱日期一、 實驗?zāi)康?) 掌握X射線衍射儀的工作原理、操作方法；2) 掌握X射線衍射實驗的樣品制備方法；3) 學(xué)會X射線衍射實驗方法、實驗參數(shù)設(shè)置，獨立完成一個衍射實驗測試；4) 學(xué)會MDI Jade 6的基本操作方法；5) 學(xué)會物相定性分析的原理和利用Jade進(jìn)行物相鑒定的方法；6) 學(xué)會物相定量分析的原理和利用Jade進(jìn)行物相定量的方法。本實驗由衍射儀操作、物相定性分析、物相定量分析三個獨立的實驗組成，實驗報告包含以

2、上三個實驗內(nèi)容。二、 實驗原理根據(jù)布拉格定律，我們可以知道，只有在特殊的入射角度時我們才能得到衍射圖像。所以，根據(jù)這一原理，我們在使用了把X射線和探測器放在環(huán)形導(dǎo)軌上的方法，把每個方向的結(jié)果都探測一遍，最終收集到能發(fā)生衍射的衍射峰。根據(jù)結(jié)果，推算晶面，判斷晶體構(gòu)型，判斷元素種類。三、 儀器與材料1) 儀器：18KW轉(zhuǎn)靶X射線衍射儀2) 數(shù)據(jù)處理軟件：數(shù)據(jù)采集與處理終端與數(shù)據(jù)分析軟件MDI Jade 63) 實驗材料： WC(碳化鎢)、LiCoOSi四、 實驗步驟1 測量數(shù)據(jù)1) 準(zhǔn)備樣品；2) 打開X射線衍射儀；3) 按下“Door”按鈕，聽到報警；4) 向右拉開“常規(guī)衍射儀門”，裝好樣品；5

3、) 向左輕拉“常規(guī)衍射儀門”，使之合上；6) 打開“控制測量”程序，輸入實驗條件和樣品名，開始測量；表1 實驗參數(shù)設(shè)定：儀器掃描范圍掃描度電壓電流D/max 2500型X射線衍射儀10-808/min 40KV250mA7) 按相同的實驗條件測量其它樣品的衍射數(shù)據(jù)。2 物相鑒定1) 打開Jade，讀入衍射數(shù)據(jù)文件；2) 鼠標(biāo)右鍵點擊S/M工具按鈕，進(jìn)入“Search/Match”對話界面;3) 選擇“Chemistry filter”，進(jìn)入元素限定對話框，選中樣品中的元素名稱，然后點擊OK返回對話框，再點擊OK；4) 從物相匹配表中選中樣品中存在的物相。在所選定的物相名稱上雙擊鼠標(biāo)，顯示PDF

4、卡片，按下Save按鈕，保存PDF卡片數(shù)據(jù)；5) 在主要相鑒定完成后，對剩余未鑒定的衍射峰涂峰，做“Search/Match”，直至全部物相鑒定出來。6) 鼠標(biāo)右鍵點擊“打印機”圖標(biāo)，顯示打印結(jié)果，按下“Save”按鈕，輸出物相鑒定結(jié)果。7) 以同樣的方法標(biāo)定其它樣品的物相,物相鑒定實驗完成。3 物相定量分析1) 在Jade窗口中，打開一個多相樣品的衍射譜；2) 完成多相樣品的物相鑒定，物相鑒定時，選擇有RIR值的PDF卡片；3) 選擇每個物相的主要未重疊的衍射峰進(jìn)行擬合，求出衍射峰面積；4) 選擇菜單“Options|Easy Quantitative”，按絕熱法計算樣品中兩相的重量百分?jǐn)?shù)；

5、5) 按下“Save”按鈕，保存定量分析結(jié)果，定量分析數(shù)據(jù)處理完成。計算公式: , 五 實驗數(shù)據(jù)處理1 物相鑒定結(jié)果2 定量分析結(jié)果（1）WCUSER: userJADE: Quantitative Analysis from Profile-Fitted PeaksDATE: Thursday, Jan 01, 2004 01:16aFILE: 005 WC.raw SCAN: 25.0/125.0/0.02/1(sec), Cu(40kV,250mA), I(max)=40668, 10-28-10 13:19PROC: New Quantitative AnalysisPhase ID

6、(2) Chemical Formula RIR Dx MAC LAC Wt% Wt(n)% Vol(n)% #L I%-I(r) Area Height Tungsten Carbide WC 15.71 15.672 161.73 2534.7 82.0 (4.2) 82.0 (4.2) 83.3 (5.7) 1 0.0 479781(21469) 30158(1046)Tungsten carbide - $-epsilon W2C 10.80 17.162 166.70 2861.0 18.0 (0.9) 18.0 (0.9) 16.7 (1.1) 1 0.0 72427(1893)

7、6967(142)2-Theta FWHM Height Height% Area(a1) Area% I(r) I(p) I%-I(r) ( h k l) 35.616 (0.004) 0.213 (0.012) 30158 (1046) 100.0 479781 (21469) 100.0 100.0 100.0 0.0 ( 1 0 0)2-Theta FWHM Height Height% Area(a1) Area% I(r) I(p) I%-I(r) ( h k l) 39.547 (0.002) 0.148 (0.005) 6967 (142) 100.0 72427 (1894)

8、 100.0 100.0 100.0 0.0 (-1-1 1)（2）LiCoOSiUSER: userJADE: Quantitative Analysis from Profile-Fitted PeaksDATE: Thursday, Jan 01, 2004 01:04aFILE: LiCoOSi (39).raw SCAN: 10.0/80.0/0.02/1(sec), Cu(40kV,250mA), I(max)=8718, 08-27-13 13:27PROC: New Quantitative AnalysisPhase ID (2) Chemical Formula RIR D

9、x MAC LAC Wt% Wt(n)% Vol(n)% #L I%-I(r) Area Height Lithium cobalt(III) oxide LiCoO2 4.38 5.049 192.28 970.8 48.3 (4.1) 48.3 (4.1) 30.1 (3.2) 1 0.0 44727(2619) 5010(263)Silicon Si 4.55 2.329 60.60 141.1 51.7 (4.4) 51.7 (4.4) 69.9 (7.5) 1 0.0 49763(3069) 6558(343)2-Theta FWHM Height Height% Area(a1)

10、Area% I(r) I(p) I%-I(r) ( h k l) 18.897 (0.005) 0.144 (0.007) 5010 (263) 100.0 44727 (2620) 100.0 100.0 100.0 0.0 ( 0 0 3)2-Theta FWHM Height Height% Area(a1) Area% I(r) I(p) I%-I(r) ( h k l) 28.409 (0.005) 0.131 (0.006) 6558 (343) 100.0 49763 (3070) 100.0 100.0 100.0 0.0 ( 1 1 1)3 點陣常數(shù)精確測定結(jié)果具體PDF卡片

11、結(jié)果：1.WCPDF#79-0743: QM=Calculated(C); d=Calculated; I=CalculatedTungsten CarbideW2 CRadiation=CuKa1Lambda=1.54060Filter=Calibration=2T=18.769-89.599I/Ic(RIR)=10.80Ref: Calculated from ICSD using POWD-12+ (1997)Hexagonal - Powder Diffraction, P-31m (162)Z=3mp=CELL: 5.19 x 5.19 x 4.724 P.S=hP9 ($GE) (

12、C5 W12)Density(c)=17.162Density(m)=17.27AMwt=379.71Vol=110.20F(23)=999.9(.0000,32/0)Ref: Epicier, T., Dubois, J., Esnouf, C., Fantozzi, G., Convert, P.Acta Metall., v36 p1903 (1988)Strong Lines: 2.27/X 2.36/2 2.60/2 1.50/2 1.35/2 1.27/2 1.75/2 1.25/1 1.14/1 1.18/1FIZ=065700: ITF TEM Mentioned.Neutro

13、n powder diffraction studies of transition metal hemicarbides M2 C1-x - II.In situ high temperature study on W2 C1-x and Mo2 C1-x k d c b a (P3-1M) NO22-Theta d(?) I(f) ( h k l) Theta 1/(2d) 2pi/d n2 18.769 4.7240 0.1 ( 0 0 1) 9.384 0.1058 1.3301 19.736 4.4947 0.1 ( 1 0 0) 9.868 0.1112 1.3979 27.366

14、 3.2563 0.1 ( 1 0 1) 13.683 0.1535 1.9296 34.535 2.5950 21.9 ( 1 1 0) 17.267 0.1927 2.4213 38.066 2.3620 23.6 ( 0 0 2) 19.033 0.2117 2.6601 39.592 2.2744 100.0 (-1-1 1) 19.796 0.2198 2.7625 43.234 2.0909 0.1 ( 1 0 2) 21.617 0.2391 3.0051 44.613 2.0294 0.1 ( 2 0 1) 22.306 0.2464 3.0961 52.332 1.7468

15、15.0 (-1-1 2) 26.166 0.2862 3.5971 56.472 1.6281 0.1 ( 2 0 2) 28.236 0.3071 3.8591 57.612 1.5986 0.1 (-2-1 1) 28.806 0.3128 3.9304 61.879 1.4982 16.2 ( 3 0 0) 30.939 0.3337 4.1938 65.281 1.4281 0.1 ( 3 0 1) 32.641 0.3501 4.3996 69.805 1.3462 15.2 (-1-1 3) 34.903 0.3714 4.6673 72.835 1.2975 2.0 ( 2 2

16、 0) 36.417 0.3854 4.8425 75.011 1.2652 15.2 ( 3 0 2) 37.505 0.3952 4.9663 75.999 1.2512 11.5 (-2-2 1) 37.999 0.3996 5.0219 79.443 1.2053 0.1 ( 3 1 1) 39.721 0.4148 5.2128 81.419 1.1810 2.1 ( 0 0 4) 40.710 0.4234 5.3202 83.670 1.1549 0.1 (-2-1 3) 41.835 0.4330 5.4406 85.272 1.1372 2.8 (-2-2 2) 42.636

17、 0.4397 5.5250 88.643 1.1025 0.1 (-3-1 2) 44.322 0.4535 5.6992 89.599 1.0932 0.1 ( 4 0 1) 44.800 0.4574 5.7477 PDF#89-2727: QM=Calculated(C); d=Calculated; I=CalculatedTungsten CarbideW CRadiation=CuKa1Lambda=1.54060Filter=Calibration=2T=31.509-84.081I/Ic(RIR)=15.71Ref: Calculated from ICSD using PO

18、WD-12+Hexagonal - Powder Diffraction, P-6m2 (187)Z=1mp=CELL: 2.906 x 2.906 x 2.837 P.S=hP2 (?)Density(c)=15.672Density(m)=15.13AMwt=195.86Vol=20.75F(9)=999.9(.0000,9/0)Ref: Parthe, E., Sadagopan, V.Monatsh. Chem., v93 p263 (1962)Strong Lines: 2.52/X 1.88/9 2.84/4 1.29/2 1.45/2 1.24/2 1.15/1 1.26/1 1

19、.42/1 0.00/1FIZ=043380: PDF 00-025-1047.M Described also as mineral from Mengyin, Shadong and Da Sichuan, China.At least one TF implausible.ITF See PDF 01-072-0097.Neutronen- und Roentgenbeugungsuntersuchungen ueber die Struktur des Wolframcarbides W C und Vergleich mit aelteren Elektronenbeugungsda

20、ten d a (P6-M2) NO2-Theta d(?) I(f) ( h k l) Theta 1/(2d) 2pi/d n2 31.509 2.8370 44.0 ( 0 0 1) 15.754 0.1762 2.2147 35.645 2.5167 100.0 ( 1 0 0) 17.823 0.1987 2.4966 48.302 1.8827 88.2 ( 1 0 1) 24.151 0.2656 3.3374 64.029 1.4530 17.9 ( 1 1 0) 32.014 0.3441 4.3243 65.780 1.4185 5.4 ( 0 0 2) 32.890 0.

21、3525 4.4295 73.113 1.2932 18.8 ( 1 1 1) 36.557 0.3866 4.8584 75.489 1.2583 9.0 ( 2 0 0) 37.745 0.3974 4.9933 77.121 1.2357 16.6 ( 1 0 2) 38.560 0.4046 5.0846 84.081 1.1503 13.9 ( 2 0 1) 42.041 0.4347 5.4624 2. LiCoOSi PDF#75-0532: QM=Calculated(C); d=Calculated; I=CalculatedLithium Cobalt OxideLi Co

22、 O2Radiation=CuKa1Lambda=1.54060Filter=Calibration=2T=18.930-87.020I/Ic(RIR)=4.38Ref: Calculated from ICSD using POWD-12+ (1997)Rhombohedral - (Unknown), R-3m (166)Z=3mp=CELL: 2.8166 x 2.8166 x 14.052 P.S=hR4 (?)Density(c)=5.049Density(m)=4.71AMwt=97.87Vol=96.54F(19)=999.9(.0000,19/0)Ref: Johnston,

23、W.D., Heikes, R.R., Sestrich, D.J. Phys. Chem. Solids, v7 p1 (1958)Strong Lines: 4.68/X 2.00/5 2.40/3 1.41/1 1.43/1 2.30/1 1.55/1 1.84/1 1.35/1 1.15/1FIZ=029225: At least one TF missing.The Preparation, Crystallography, and Magnetic Properties of the Lix Co1-x O System h b a (R3-MH) ABX22-Theta d(?)

24、 I(f) ( h k l) Theta 1/(2d) 2pi/d n2 18.930 4.6840 100.0 ( 0 0 3) 9.465 0.1067 1.3414 37.387 2.4033 28.8 ( 1 0 1) 18.694 0.2080 2.6144 38.404 2.3420 3.7 ( 0 0 6) 19.202 0.2135 2.6828 39.057 2.3043 9.2 ( 0 1 2) 19.528 0.2170 2.7267 45.219 2.0036 51.9 ( 1 0 4) 22.609 0.2495 3.1359 49.435 1.8421 7.7 (

25、0 1 5) 24.717 0.2714 3.4108 59.122 1.5613 1.0 ( 0 0 9) 29.561 0.3202 4.0243 59.597 1.5500 8.4 ( 1 0 7) 29.798 0.3226 4.0536 65.422 1.4254 10.4 ( 0 1 8) 32.711 0.3508 4.4080 66.317 1.4083 10.7 ( 1 1 0) 33.159 0.3550 4.4615 69.660 1.3487 6.7 ( 1 1 3) 34.830 0.3707 4.6588 78.487 1.2176 1.2 ( 1 0 10) 39

26、.243 0.4106 5.1603 78.683 1.2151 2.0 ( 0 2 1) 39.342 0.4115 5.1711 79.320 1.2069 1.8 ( 1 1 6) 39.660 0.4143 5.2061 79.736 1.2017 0.9 ( 2 0 2) 39.868 0.4161 5.2288 82.264 1.1710 1.2 ( 0 0 12) 41.132 0.4270 5.3657 83.911 1.1522 3.8 ( 0 2 4) 41.955 0.4340 5.4534 85.791 1.1317 2.1 ( 0 1 11) 42.896 0.441

27、8 5.5522 87.020 1.1188 0.8 ( 2 0 5) 43.510 0.4469 5.6160 PDF#89-2955: QM=Calculated(C); d=Calculated; I=CalculatedSiliconSiRadiation=CuKa1Lambda=1.54060Filter=Calibration=2T=28.445-88.041I/Ic(RIR)=4.55Ref: Calculated from ICSD using POWD-12+Cubic - (Unknown), Fd-3m (227)Z=8mp=CELL: 5.43029 x 5.43029

28、 x 5.43029 P.S=cF8 (?)Density(c)=2.330Density(m)=2.329Mwt=28.09Vol=160.13F(7)=999.9(.0000,7/0)Ref: Straumanis, M.E., Borgeaud, P., James, W.J.J. Appl. Phys., v32 p1382 (1961)Strong Lines: 3.14/X 1.92/6 1.64/3 1.11/1 1.25/1 1.36/1 1.57/1 0.00/1 0.00/1 0.00/1FIZ=043610: M Measured at unetched crystal

29、fragments.M Cell for etched crystal bar: 5.43048 (Dm=2.3289).M Cell for powder, unheated: 5.43081.M Cell for powder, heated: 5.43070.M PDF 00-027-1402.No R value given.At least one TF missing.See PDF 01-075-0589.Perfection of the lattice of dislocation-free silicon, studies by the lattice-constant a

30、nd density method a (FD3-MS) N2-Theta d(?) I(f) ( h k l) Theta 1/(2d) 2pi/d n2 28.445 3.1352 100.0 ( 1 1 1) 14.223 0.1595 2.0041 3 47.307 1.9199 55.4 ( 2 2 0) 23.654 0.2604 3.2727 8 56.128 1.6373 30.0 ( 3 1 1) 28.064 0.3054 3.8376 11 58.862 1.5676 0.1 ( 2 2 2) 29.431 0.3190 4.0082 12 69.138 1.3576 6

31、.9 ( 4 0 0) 34.569 0.3683 4.6283 16 76.385 1.2458 9.5 ( 3 3 1) 38.193 0.4014 5.0435 19 88.041 1.1085 11.5 ( 4 2 2) 44.021 0.4511 5.6684 24六 結(jié)果與討論一、實驗原理本次實驗采用的儀器為X射線衍射儀，它是按照晶體對X射線衍射的幾何原理設(shè)計制造的。布拉格方程是X射線衍射儀最基本的理論基礎(chǔ)，也是進(jìn)行X射線檢測最根本和重要的理論依據(jù)之一。由知，確定了一組相互對應(yīng)的與便可求出一組干涉面的面間距d，當(dāng)干涉指數(shù)互質(zhì)時，干涉面就代表一族真實的晶面。因為存在系統(tǒng)消光，并非所有滿足布拉格方程的干涉面都有對應(yīng)的衍射條紋。為保證能得到足夠的衍射譜線以分析，X射線衍射儀使用的是粉末樣品，用單色（標(biāo)識）X射線照射多晶體試樣，即多晶體衍射方法，并且同時使樣品轉(zhuǎn)動（-2連動），設(shè)計2:1的角速度比，目的是確保探測的衍射線與入射線始終保持2的關(guān)系，即入射線與衍射線以試樣表面法線為對稱軸，在兩側(cè)對稱分布；輻射探測器接收到的衍射是那些與試