X射线衍射实验报告

1、中南大学X射线衍射实验报告实验目的材料科学与工程学院材料国际专业学号06051401181401班级同组者姓名蔡云伟实验日期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。二、

2、实验原理feorMH X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专靶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“常规衍

3、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10-808min：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OK4）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Save按钮，保存

4、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“ Save”按钮，保存定量分析

5、结果，定量分析数据处理完成。 计算公式：KbaaAI2O3K bK A12O3RIRaRIRbWaIa(IaIbK：)五实验数据处理1物相鉴定结果eurtoCJx卫邕-40.Q-3= n-3D.L-25.Q-2QQ-15.il-10.050=IDS.too 忧讪3040TSvo-Pieta (da 曲UQ11090 1W75un-1. i ?Sii m1020TW耐（a|d砌500(wLmull-IAlHu&LI-II5-2O2定量分析结果(1) WCUSER: userJADE: Qua ntitative An alysis from Profile-Fitted PeaksDATE: T

6、hursday, Jan 01,2004 01:16aFILE: 005 WC.rawl(max)=40668.SCAN: 25.0/125.0/0.02/1(sec),Cu(40kV,250mA),10-28-10 13:19PROC: New Qua ntitative An alysisMACLACWt%Wt(n)%Vol( n)%Area HeightTun gste n CarbideWC15.7115.672161.732534.782.0(4.2)82.0(4.2)83.3(5.7)479781(21469) 30158(1046)Tun gste n carbide - $-e

7、psil on W2C10.80 17.162166.702861.018.0(0.9)18.0(0.9)16.7(1.1)72427(1893)6967(142)Phase ID Chemical Formula RIR Dx#L I%-I(r)10.010.02-ThetaFWHMHeight 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-ThetaFWHM He

8、ight 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 0.0 (-1-1 1)(2) LiCoOSiUSER: userJADE: Qua ntitative An alysis from Profile-Fitted PeaksDATE: Thursday, Jan 01,2004 01:04aFILE: LiCoOSi (39).rawSCAN: 10.0/80.0/0.02/1(sec),

9、 Cu(40kV,250mA), I(max)=8718, 08-27-1313:27PROC: New Quantitative AnalysisPhase ID (2)Chemical Formula RIR Dx MACLAC Wt% Wt(n)% Vol( n)% #L I%-I(r) Area HeightLithium cobalt(III) oxide LiCoO2 4.38 5.049 192.28970.8 48.3 (4.1) 48.3 (4.1) 30.1 (3.2) 10.0 44727(2619)5010(263)Silic onSi4.55 2.329 60.601

10、41.1 51.7 (4.4) 51.7 (4.4) 69.9 (7.5) 10.0 49763(3069)6558(343)2-ThetaFWHM Height Height% Area(a1)Area% I(r) I(p) l%-l(r) ( h k l)18.897 (0.005) 0.144 (0.007) 5010 (263)100.0 44727 (2620)100.0 100.0 100.00.0 ( 0 0 3)2-ThetaFWHM Height Height% Area(a1)Area% I(r) I(p) I%-I(r) ( h k l)28.409 (0.005) 0.

11、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 Tun gsten Carbide - WC W2C Tun gsten Carbide=82.0%Quan titative An alysis from Profile-Fitted PeaksLiCoO2 I I Silicon - Si Silicon=51.7%Quan titative An alysis from Profile-Fitted Peaks具体PDF卡片结果：1. WCPDF#79-0743: QM=Ca

12、lculated(C); d=Calculated; l=CalculatedTun gste n CarbideW2 CRadiatio n=CuKa1 Lambda=1.54060 Filter=Calibrati on=2T=18.769-89.599l/lc(RIR)=10.80Ref: Calculated from ICSD usi ng POWD-12+ (1997)Hexago nal - Powder Diffractio n, P-31m (162)Z=3 mp=CELL: 5.19 x 5.19 x 4.724 P.S=hP9 ($GE) (C5 W12)Den sity

13、(c)=17.162Den sity(m)=17.27AMwt=379.71 Vol=110.20F(23)=999.9(.0000,32/0)Ref: Epicier, T., Dubois, J., Esnouf, C., Fan tozzi, 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 1.14/11.18/1FIZ=065700: ITF TEM Me ntio ned.Neutr on powder

14、diffracti on studies of tran siti on 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 nA218.7694.72400.1(0 0 1) 9.384 10.10581.330119.7364.49470.1(1 0 0) 9.868 10.11121.397927.3663.25630.1(1 0 1) 1

15、3.6830.15351.929634.5352.595021.9(1 1 0) 17.2670.19272.421338.0662.362023.6(0 0 2) 19.0330.21172.660139.5922.2744100.0 (-1-1 1) 19.796 0.2198 2.762543.2342.09090.1(1 0 2) 21.6170.23913.005144.6132.02940.1(2 0 1) 22.3060.24643.096152.3321.746815.0(-1-1 2) 26.1660.28623.597156.4721.62810.1(2 0 2) 28.2

16、360.30713.859157.6121.59860.1(-2-1 1) 28.8060.31283.930461.8791.498216.2(3 0 0) 30.9390.33374.193865.2811.42810.1(3 0 1) 32.6410.35014.399669.8051.346215.2(-1-1 3) 34.9030.37144.667372.8351.29752.0(2 2 0) 36.4170.38544.842575.0111.265215.2(3 0 2) 37.5050.39524.966375.9991.251211.5(-2-2 1) 37.9990.39

17、965.021979.4431.20530.1(3 1 1) 39.7210.41485.212881.4191.18102.1(0 0 4) 40.7100.42345.320283.6701.15490.1(-2-1 3) 41.8350.43305.440685.2721.13722.8(-2-22)42.6360.43975.525088.6431.10250.1(-3-12)44.3220.45355.699289.5991.09320.1( 4 01)44.8000.45745.7477PDF#89-2727: QM=Calculated(C); d=Calculated; l=C

18、alculatedTun gste n CarbideW CRadiatio n=CuKa1 Lambda=1.54060 Filter=Calibratio n=2T=31.509-84.081I/Ic(RIR)=15.71Ref: Calculated from ICSD us ing POWD-12+Hexago nal - Powder Diffractio n, P-6m2 (187)Z=1 mp=CELL: 2.906 x 2.906 x 2.837 P.S=hP2 (?)Den sity(c)=15.672Den sity(m)=15.13AMwt=195.86 Vol=20.7

19、5F(9)=999.9(.0000,9/0)Ref: Parthe, E., Sadagopa n, V.Mon atsh. 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 00-025-1047.M Described also as min eral from Mengyin, Shad ong and Da Sichua n, Ch ina. At least one TF implausible

20、.Struktur des d a (P6-M2)ITF See PDF 01-072-0097.Neutr onen-und Roen tge nbeugu ngsun tersuchu ngenueber dieWolframcarbides WC und Vergleich mit aelterenElektronenbeugungsdatenNO2-Thetad(?) I(f) ( h k l) Theta 1/(2d) 2pi/d n231.509 2.837035.645 2.516748.302 1.882764.029 1.453065.780 1.418573.113 1.2

21、93275.489 1.258377.121 1.235784.081 1.150344.0 ( 0 0 1) 15.754 0.1762 2.2147100.0 ( 1 0 0) 17.823 0.1987 2.496688.2 ( 1 0 1) 24.151 0.2656 3.337417.9 ( 1 1 0) 32.014 0.3441 4.32435.4 ( 0 0 2) 32.890 0.3525 4.429518.8 ( 1 1 1) 36.557 0.3866 4.85849.0 ( 2 0 0) 37.745 0.3974 4.993316.6 ( 1 0 2) 38.560

22、0.4046 5.084613.9 ( 2 0 1) 42.041 0.4347 5.46242. LiCoOSiPDF#75-0532: QM=Calculated(C); d=Calculated; I=CalculatedLithium Cobalt OxideLi Co O2Radiatio n=CuKa1 Lambda=1.54060 Filter=Calibrati on=2T=18.930-87.020l/lc(RIR)=4.38Ref: Calculated from ICSD usi ng P0WD-12+ (1997)Rhombohedral - (Unknown), R-

23、3m (166)Z=3 mp=CELL: 2.8166 x 2.8166 x 14.052 P.S=hR4 (?)Den sity(c)=5.049Den sity(m)=4.71AMwt=97.87Vol=96.54F(19)=999.9(.0000,19/0)Ref: Johnston, 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 1.41/11.43/1 2.30/11.55/11.84/1 1.35/11.15/1FIZ=029

24、225: At least one TF missing.The Preparation,Crystallography, and Magnetic Properties of the Lix Co1-x O Systemh b a (R3-MH) ABX22-Thetad(?)I(f) ( h k l) Theta 1/(2d) 2pi/d nA218.9304.6840100.0 ( 0 0 3)9.4650.10671.341437.3872.403328.8(1 0 1)18.6940.20802.614438.4042.34203.7(0 0 6)19.2020.21352.6828

25、39.0572.30439.2(0 1 2)19.5280.21702.726745.2192.003651.9(1 0 4)22.6090.24953.135949.4351.84217.7(0 1 5)24.7170.27143.410859.1221.56131.0(0 0 9)29.5610.32024.024359.5971.55008.4(1 0 7)29.7980.32264.053665.4221.425410.4(0 1 8)32.7110.35084.408066.3171.408310.7(1 1 0)33.1590.35504.461569.6601.34876.7(1

26、 1 3)34.8300.37074.658878.4871.21761.2(1 0 10)39.2430.41065.160378.6831.21512.0(0 2 1)39.3420.41155.171179.3201.20691.8(1 1 6)39.6600.41435.206179.7361.20170.9(2 0 2)39.8680.41615.228882.2641.17101.2(0 0 12)41.1320.42705.365783.9111.15223.8(0 2 4)41.9550.43405.453485.7911.13172.1(0 1 11)42.8960.4418

27、5.552287.0201.11880.8(2 0 5)43.5100.44695.6160PDF#89-2955: QM=Calculated(C); d=Calculated; I=CalculatedSilico nSiRadiatio n=CuKa1 Lambda=1.54060 Filter=Calibratio n=2T=28.445-88.041I/Ic(RIR)=4.55Ref: Calculated from ICSD us ing POWD-12+Cubic - (Unknown), Fd-3m (227) Z=8 mp=CELL: 5.43029 x 5.43029 x

28、5.43029 P.S=cF8 (?)Den sity(c)=2.330De nsity(m)=2.329Mwt=28.09Vol=160.13F=999.9(.0000,7/0)Ref: Strauma nis, M.E., Borgeaud, P., James, W.J.J. Appl. Phys., v32 p1382 (1961)Strong Lines: 3.14/X 1.92/6 1.64/3 1.11/11.25/11.36/11.57/10.00/1 0.00/10.00/1FIZ=043610: M Measured at un etched crystal fragme

29、nts.M Cell for etched crystal bar: 5.43048 (Dm=2.3289).M Cell for powder, un heated: 5.43081.M Cell for powder, heated: 5.43070.M PDF 00-027-1402.No R value give n.At least one TF miss ing.See PDF 01-075-0589.Perfecti on of the lattice ofdislocati on-freesilic on,studies by thelattice-co nsta nt and

30、 den sity method a (FD3-MS) N 2-Theta d(?) I(f) ( h k l) Theta 1/(2d) 2pi/d n228.445 3.135247.307 1.919956.128 1.637358.862 1.567669.138 1.357676.385 1.245888.041 1.1085100.0 ( 1 1 1) 14.223 0.1595 2.0041355.4 ( 2 2 0) 23.654 0.2604 3.2727830.0 ( 3 1 1) 28.064 0.3054 3.8376 110.1 ( 2 2 2) 29.431 0.3

31、190 4.0082 126.9 ( 4 0 0) 34.569 0.3683 4.6283 169.5 ( 3 3 1) 38.193 0.4014 5.0435 1911.5 ( 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2dsin n知，确定了一组相互对应的B与入便可 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 （9 -2 B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29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行的晶面产生的衍射；同样的晶面若不平行于试样表面，即使产生衍射，其衍射线进不了探测器，不能被接受；X射线源由X射线发生器产生，其线状焦点位于测角仪周围位置上固定不动。在线 状焦