X射线衍射实验报告

1、.中 南 大 学X射线衍射实验报告材料科学与工程学院材料国际专业1401班级姓 名蔡云伟学号18同组者 实验日期2016年05月18日指导教师黄继武评分分评阅人评阅日期一、 实验目的1) 掌握X射线衍射仪的工作原理、操作方法；2) 掌握X射线衍射实验的样品制备方法；3) 学会X射线衍射实验方法、实验参数设置，独立完成一个衍射实验测试；4) 学会MDI Jade 6的基本操作方法；5) 学会物相定性分析的原理和利用Jade进行物相鉴定的方法；6) 学会物相定量分析的原理和利用Jade进行物相定量的方法。本实验由衍射仪操作、物相定性分析、物相定量分析三个独立的实验组成，实验报告包含以上三个实验内容

2、。二、 实验原理根据布拉格定律，我们可以知道，只有在特殊的入射角度时我们才能得到衍射图像。所以，根据这一原理，我们在使用了把X射线和探测器放在环形导轨上的方法，把每个方向的结果都探测一遍，最终收集到能发生衍射的衍射峰。根据结果，推算晶面，判断晶体构型，判断元素种类。三、 仪器与材料1) 仪器：18KW转靶X射线衍射仪2) 数据处理软件：数据采集与处理终端与数据分析软件MDI Jade 63) 实验材料： WC(碳化钨)、LiCoOSi四、 实验步骤1 测量数据1) 准备样品；2) 打开X射线衍射仪；3) 按下“Door”按钮，听到报警；4) 向右拉开“常规衍射仪门”，装好样品；5) 向左轻拉“

3、常规衍射仪门”，使之合上；6) 打开“控制测量”程序，输入实验条件和样品名，开始测量；表1 实验参数设定：仪器扫描范围扫描度电压电流D/max 2500型X射线衍射仪10-808/min 40KV250mA7) 按相同的实验条件测量其它样品的衍射数据。2 物相鉴定1) 打开Jade，读入衍射数据文件；2) 鼠标右键点击S/M工具按钮，进入“Search/Match”对话界面;3) 选择“Chemistry filter”，进入元素限定对话框，选中样品中的元素名称，然后点击OK返回对话框，再点击OK；4) 从物相匹配表中选中样品中存在的物相。在所选定的物相名称上双击鼠标，显示PDF卡片，按下Sa

4、ve按钮，保存PDF卡片数据；5) 在主要相鉴定完成后，对剩余未鉴定的衍射峰涂峰，做“Search/Match”，直至全部物相鉴定出来。6) 鼠标右键点击“打印机”图标，显示打印结果，按下“Save”按钮，输出物相鉴定结果。7) 以同样的方法标定其它样品的物相,物相鉴定实验完成。3 物相定量分析1) 在Jade窗口中，打开一个多相样品的衍射谱；2) 完成多相样品的物相鉴定，物相鉴定时，选择有RIR值的PDF卡片；3) 选择每个物相的主要未重叠的衍射峰进行拟合，求出衍射峰面积；4) 选择菜单“Options|Easy Quantitative”，按绝热法计算样品中两相的重量百分数；5) 按下“S

5、ave”按钮，保存定量分析结果，定量分析数据处理完成。计算公式: , 五 实验数据处理1 物相鉴定结果2 定量分析结果（1）WCUSER: userJADE: Quantitative Analysis from Pro 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 (2) Chemical Formu

6、la 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) 6967(142)2-Theta F

7、WHM 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) 100.0 100.0 100.0

8、 0.0 (-1-1 1)（2）LiCoOSiUSER: userJADE: Quantitative Analysis from Pro 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 Dx MAC LAC Wt% Wt(n)% Vol(n)%

9、#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) Area% I(r) I(p) I%-I(r) ( h k

10、 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 点阵常数精确测定结果具体PDF卡片结果：1.WCPDF#79-0743: QM=Calcul

11、ated(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) (C5 W12)Density(c)=17.162Densi

12、ty(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.Neutron powder diffraction studies

13、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 3.2563 0.1 ( 1 0 1) 13.683 0

14、.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 15.0 (-1-1 2) 26.166 0.2862 3

15、.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 0) 36.417 0.3854 4.8425 75.0

16、11 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 0.4397 5.5250 88.643 1.1025

17、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 POWD-12+Hexagonal - Powder Diff

18、raction, 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 1.42/1 0.00/1FIZ=043380: PDF 0

19、0-025-1047.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 Elektronenbeugungsdaten d a (P6-M2) NO2-Theta d(?

20、) 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 0.3525 4.4295 73.113 1.2932 18.

21、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 O2Radiation=CuKa1Lambda=1.54

22、060Filter=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, W.D., Heikes, R.R., Sestrich,

23、 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(?) I(f) ( h k l) Theta 1/(2d) 2

24、pi/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 ( 0 1 5) 24.717 0.2714 3.4108 5

25、9.122 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) 39.243 0.4106 5.1603 78.683 1.2

26、151 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 0.4418 5.5522 87.020 1.1188 0.8 (

27、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 x 5.43029 P.S=cF8 (?)Density

28、(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 fragments.M Cell for etched c

29、rystal 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 and density method a (FD3-MS)

30、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 6.9 ( 4 0 0) 34.569 0.3683 4.6

31、283 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 结果与讨论一、实验原理本次实验采用的仪器为X射线衍射仪，它是按照晶体对X射线衍射的几何原理设计制造的。布拉格方程是X射线衍射仪最基本的理论基础，也是进行X射线检测最根本和重要的理论依据之一。由知，确定了一组相互对应的与便可求出一组干涉面的面间距d，当干涉指数互质时，干涉面就代表一族真实的晶面。因为存在系统消光，并非所有满足布拉格方程的干涉面都有对应的衍射条纹。为保证能得到足够的衍射谱线以分析，X射线衍射仪使用的是粉末样品，用单色（标识）X射线照射多晶体试样，即多晶体衍射方法，并且同时使样品转动（-2连动），设计2:1的角速度比，目的是确保探测的衍射线与入射线始终保持2的关系，即入射线与衍射线以试样表面法线为对称轴，在两侧对称分布；辐射探测器接收到的衍射是那些与试样表面平