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 日指导教师评分分评阅人评阅日期班级黄继武31)2)3)4)5)6),1*0 "咏I ' 实验目的掌握X射线衍射仪的工作原理、操作方法；掌握X射线衍射实验的样品制备方法；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;学会MDI Jade 6的基本操作方法；学会物相定性分析的原理和利用 Jade进行物相鉴定的方法； 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

2、报告包含以上三个实验内容。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。仪器与材料1)2)3)四、仪器：18KW专靶X射线衍射仪数据处理软件：数据采集与处理终端与数据分析软件MDI Jade 6实验材料：WC碳化钨）、LiCoOSi实验步骤1测量数据1)2)3)4)5)6)准备样品；打开X射线衍射仪；按下“ Door”按钮，听到报警；向右拉开“常规衍射仪门”，装好样品；向左轻拉

3、“常规衍射仪门”，使之合上；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：2物相鉴定 打开Jade，读入衍射数据文件；鼠标右键点击S/M工具按钮，进入“ Search/Match ”对话界面；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PDF卡片数据；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。鼠标右键点击“打印机”图标，显示打

4、印结果，按下“Save”按钮，输出物相鉴定结果。以同样的方法标定其它样品的物相，物相鉴定实验完成。1)2)3)4)5)6)7)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°min40KV250mA7）按相同的实验条件测量其它样品的衍射数据。1)2)3)4)3物相定量分析在Jade窗口中，打开一个多相样品的衍射谱；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；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；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

5、钮，保存定量分析结果，定量分析数据处理完成。计算公式：IX a K A12O3Kb -bK AI2O3RIRaIRRb，Wa aIbK：)五实验数据处理1物相鉴定结果5.03040jOo o o 氐 o m2 2 1 (巴UnQu芝mu哲匸一JjL50eu39-27rTi Tu-尸利 Cnijk'' 瞅® Ci<) ：> n 羽A ¥<?Pn 初Qi r ztri de - £-曰厂临p 1 0-)u A M1 £100no120-unzoz-McatLI-52定量分析结果(1) WCUSER: userJADE: Qu

6、an titative An alysis from Pro P eaksDATE: Thursday, Jan 01,2004 01:16aFILE: 005 WC.rawCu(40kV,250mA),l(max)=40668.SCAN: 25.0/125.0/0.02/1(sec),10-28-10 13:19P ROC: New Qua ntitative An alysis16P hase ID (2) MAC LAC Area HeightTun gste n Carbide161.732534.782.0Chemical Formula RIRWt%Wt(n)%DxVol( n)%

7、#Ll%-l(r)WC(4.2)82.015.71(4.2)15.67283.3 (5.7)0.0479781(21469) 30158(1046)Tun gste n carbide - $-e psil on 166.702861.018.0 (0.9)72427(1893)6967(142)W2C18.0(0.9)10.80 17.16216.7 (1.1)0.0FWHMHeight2-ThetaArea(a1) Area% I(r) l(p) I%-I(r) ( h k l)0.213(0.012) 30158(1046)100.0 4797810.0 ( 1 0 0)35.616 (

8、0.004)100.0 100.0 100.0Height%(21469)FWHM Height Height% Area(a1)2-ThetaArea% I(r) l(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: Quan titative An alysis from Pro P eaksDATE: Thursday, Jan 01,2004 01:04aFILE: LiC

9、oOSi (39).rawSCAN: 10.0/80.0/0.02/1(sec), Cu(40kV,250mA), I(max)=8718, 08-27-1313:27P ROC: New Qua ntitative An alysisP hase ID (2)Chemical Formula RIR Dx MACLAC Wt%Wt( n)% Vol( n)% #L l%-l(r) AreaHeightLithium cobalt(lll) oxide LiCoO2 4.38 5.049 192.28 970.8 48.3 (4.1) 48.3 (4.1) 30.1 (3.2) 10.0 44

10、727(2619)5010(263)Silic on141.1 51.7 (4.4)6558(343)Si4.55 2.329 60.6051.7 (4.4) 69.9 (7.5) 10.0 49763(3069)FWHM Height Height% Area(a1)2-ThetaArea% I(r) l(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%

11、 I(r) l(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 Tun gsten Carbide - WC <Wt%=82.0 (4.2)> W2C <Wt%=18.0 (0.9)>Tun gsten Carbide=82.0%Quan titative An alysis from Profile-Fitted P eaks口 LiCoO2 <Wt%=48.3 (4.1)&g

12、t; Silicon - Si <Wt%=51.7 (4.4)>Wt%Silico n二 51.7%Quan titative An alysis from Profile-Fitted Peaks具体PDF卡片结果:1.WCP DF#79-0743: QM=Calculated(C); d=Calculated; l=CalculatedTun gste n CarbideW2 CRadiati on=CuKa1 Lambda=1.54060 Filter=Calibratio n=2T=18.769-89.599l/lc(RIR)=10.80Ref: Calculated fr

13、om ICSD usi ng PO WD-12+ (1997)Z=3 mp=P .S=h P9 ($GE) (C5 W12)Mwt=379.71Vol=110.20Hexago nal - Powder Diffractio n, P-31m (162)CELL: 5.19 x 5.19 x 4.724 <90.0 x 90.0 x 120.0>Den sity(c)=17.162 De nsity(m)=17.27AF(23)=999.9(.0000,32/0)Ref: Ep icier, T., Dubois, J., Esnouf, C., Fan tozzi, G., Co

14、nvert, P.Acta Metall., v36 p1903 (1988)Stro ng Lin es: 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 po wder diffracti on studies of tran siti on metal hemicarbides M2 C1-x-II.In situ high temp erature study on W2 C1-x and Mo2 C1-x k d c

15、 b a (P 3-1M) NO218.7694.72400.1(0 0 1)9.384 10.10581.330119.7364.49470.1(1 0 0)9.868 <0.11121.397927.3663.25630.1(1 0 1)13.6830.15351.929634.5352.595021.9(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

16、.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)28.2360.30713.859157.6121.59860.1(-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

17、.8351.29752.0(2 2 0)36.4170.3854 4.842575.0111.265215.2(3 0 2) 37.5050.39524.966375.9991.251211.5(-2-2 1) 37.9990.39965.021979.4431.20530.1(3 1 1)39.7210.41485.212881.4191.18102.1(0 0 4)40.7100.42345.320283.6701.15490.1(-2-1 3)41.8350.43305.4406d 1(f) ( h k I) Theta 1/(2d) 2pi/d 门人22-Theta85.272 1.1

18、37288.643 1.102589.599 1.09322.8 (-2-2 2) 42.636 0.4397 5.52500.1 (-3-1 2) 44.322 0.4535 5.69920.1 ( 4 0 1) 44.800 0.4574 5.7477P DF#89-2727: QM=Calculated(C); d=Calculated; I=CalculatedTun gste n CarbideRadiati on=CuKa1 Lambda=1.54060 Filter=Calibratio n=2T=31.509-84.081I/Ic(RIR)=15.71Ref: Calculat

19、ed from ICSD us ing PO WD-12+Hexago nal - Powder Diffractio n, P-6m2 (187)CELL: 2.906 x 2.906 x 2.837 <90.0 x 90.0 x 120.0>Z=1mp=P.S=h P2 (?)Den sity(c)=15.672 De nsity(m)=15.13AF(9)=999.9(.0000,9/0)Ref: P arthe, E., Sadago pan, V.Mwt=195.86Vol=20.75Mon atsh. Chem., v93 p263 (1962)Stro ng Lin

20、es: 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 imp lausible.ITF See PDF 01-072-0097.Neutr onen- und Roen tge nbeugu ngsun tersuchu ngenueber die Struktur

21、 desWolframcarbides WC und Vergleich mit aelteren Elektronenbeugungsdaten d a (P6-M2) NO2-Theta31.509d(?) I(f) ( h k l) Theta 1/(2d) 2pi/d 门人22.837035.6452.516748.3021.882744.0 ( 0 0 1) 15.754 0.1762 2.2147100.0 ( 1 0 0) 17.823 0.1987 2.496688.264.0291.453017.965.7801.41855.4(1 0 1)(1 1 0)(0 0 2)24.

22、15132.01432.89073.1131.293218.875.4891.25839.077.1211.235716.684.0811.150313.9(1 1 1) (2 0 0)(1 0 2)(2 0 1)36.55737.74538.56042.0410.2656 3.33740.3441 4.32430.3525 4.42950.3866 4.85840.3974 4.99330.4046 5.08460.4347 5.46242. LiCoOSiPDF#75-0532: QM=Calculated(C); d=Calculated; I=Calculated Lithium Co

23、balt OxideLi Co O2Radiatio n=CuKa1 Lambda=1.54060Filter=Calibratio n=2T=18.930-87.020I/Ic(RIR)=4.38Ref: Calculated from ICSD us ing PO WD-12+ (1997)Rhombohedral - (Unknown), R-3m (166)Z=3 mp=CELL: 2.8166 x 2.8166 x 14.052 <90.0 x 90.0 x 120.0>Mwt=97.87Den sity(c)=5.049Den sity(m)=4.71AF(19)=99

24、9.9(.0000,19/0)Ref: Joh nsto n, W.D., Heikes, R.R., Sestrich, D.J. P hys. Chem. Solids, v7 p1 (1958)Strong Lines: 4.68/X 2.00/5 2.40/3 1.41/11.43/1 2.30/1FIZ=029225: At least o ne TF missi ng.The Preparation,Crystallography,and Magnetic Propertiesh b a (R3-MH) ABX2P. S=hR4 (?)Vol=96.541.55/11.84/1 1

25、.35/11.15/1of the Lix Co1-x O System2-Thetad(?)I(f) ( h k l) Theta 1/(2d) 2pi/d n218.9304.6840100.0 ( 0 0 3)9.4650.10671.341437.3872.403328.8 ( 1 0 1)18.6940.20802.614438.4042.34203.7 ( 0 0 6)19.2020.21352.682839.0572.30439.2 ( 0 1 2)19.5280.21702.726745.2192.003651.9 ( 1 0 4)22.6090.24953.135949.43

26、51.84217.7(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 1 3)34.8300.37074.658878.4871.21761.2(1 0 10)39.2430.41065.160378.6831.21512.0(

27、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)42.8960.44185.552287.0201.11880.8(2 0 5)43.5100.44695.6160P DF#89-2955: QM=Calculated(C); d=

28、Calculated; l=CalculatedSilico nSiRadiatio n=CuKa1 Lambda=1.54060Filter=Calibrati on=2T=28.445-88.041I/Ic(RIR)=4.55Ref: Calculated from ICSD us ing PO WD-12+Cubic - (Unknown), Fd-3m (227) Z=8 mp=P.S=cF8 (?)CELL: 5.43029 x 5.43029 x 5.43029 <90.0 x 90.0 x 90.0>Mwt=28.09Vol=160.13Den sity(c)=2.3

29、30Den sity(m)=2.329F=999.9(.0000,7/0)Ref: Strauma nis, M.E., Borgeaud, P., James, W.J.0.00/1 0.00/1 0.00/1J. App I. P hys., v32 p1382 (1961)Strong Lines: 3.14/X 1.92/6 1.64/3 1.11/11.25/11.36/11.57/1FIZ=043610: M Measured at un etched crystal fragme nts.M Cell for etched crystal bar: 5.43048 (Dm=2.3

30、289).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.silic on.studies by thePerfecti onof the lattice ofdislocati on-freelattice-co nsta nt and den sity method a (FD3-MS) N2-Theta28.44547.30756.

31、12858.86269.13876.385d(?) 1(f) ( h k l) Theta 1/(2d) 2pi/d 门人2 3.1352 1.9199 1.63731.56761.35761.245888.0411.1085100.0 ( 1 1 1) 14.223 0.1595 2.004155.4 ( 2 2 0) 23.654 0.2604 3.2727 30.0 ( 3 1 1) 28.064 0.3054 3.8376 0.1 ( 2 2 2) 29.4316.9 ( 4 0 0) 34.5699.5 ( 3 3 1) 38.19311.5 ( 4 2 2) 44.0210.319

32、0 4.00820.3683 4.62830.4014 5.04350.4511 5.6684381112161924六结果与讨论一、实验原理X射线衍射的几何原本次实验采用的仪器为X射线衍射仪，它是按照晶体对理设计制造的。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0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 （0 -2 0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20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