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0605140118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

2、验组成，实验报告包含以上三个实验内容。二、实验原理精品资料_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；精品资料_3) 按下“Door ”按

3、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°/min40KV250mA7) 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，

4、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 Save 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。精品资料_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

5、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，保存定量分析结果，定量分析数据处理完成。计算公式 :aKK baRIRaI aAl 2O 3, WabRIRbaAl 2O 3(I aIb Kb )五 实验数据处理1 物相鉴定结果精品资料_2 定量分析结果（1）WC USER: userJADE: Quantitative Analysis from Profile-Fitted Peaks精品资料_DATE: Thursday, Jan 01, 2004 01:16aFILE

6、: 005 WC.rawSCAN: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 FormulaRIRDxMACLACWt%Wt(n)%Vol(n)% #LI%-I(r)AreaHeightTungstenCarbideWC15.7115.672161.732534.782.0(4.2)82.0(4.2)83.3(5.7)10.0479781(21469)30158(1046)Tungstencarbide -$

7、-epsilon W2C10.8017.162166.702861.018.0(0.9)18.0(0.9)16.7(1.1)10.072427(1893)6967(142)2-ThetaFWHMHeightHeight%Area(a1) Area%I(r)I(p)I%-I(r) ( h k l)35.616 (0.004)0.213(0.012)30158 (1046)100.0479781 (21469)100.0 100.0 100.00.0(100)2-ThetaFWHMHeightHeight%精品资料_Area(a1)Area%I(r) I(p)I%-I(r)( h k l)39.5

8、47(0.002)0.148(0.005)6967(142)100.072427(1894)100.0 100.0 100.00.0(-1-1 1)（2）LiCoOSiUSER: userJADE: Quantitative Analysis from Profile-Fitted PeaksDATE: Thursday, Jan 01, 2004 01:04aFILE: LiCoOSi (39).rawSCAN: 10.0/80.0/0.02/1(sec),Cu(40kV,250mA),I(max)=8718,08-27-1313:27PROC: New Quantitative Analy

9、sisPhase ID (2)ChemicalFormulaRIRDxMACLACWt%Wt(n)%Vol(n)%#LI%-I(r)AreaHeightLithiumcobalt(III) oxideLiCoO24.38 5.049192.28970.848.3(4.1)48.3(4.1)30.1(3.2)10.044727(2619)5010(263)SiliconSi4.552.32960.60141.151.7(4.4)51.7(4.4)69.9(7.5)10.049763(3069)6558(343)精品资料_2-ThetaFWHMHeightHeight%Area(a1)Area%I

10、(r) I(p)I%-I(r)( h k l)18.897(0.005)0.144(0.007)5010(263)100.044727(2620)100.0 100.0 100.00.0(003)2-ThetaFWHMHeightHeight%Area(a1)Area%I(r) I(p)I%-I(r)( h k l)28.409(0.005)0.131(0.006)6558(343)100.049763(3070)100.0 100.0 100.00.0( 11 1)3 点阵常数精确测定结果Tungsten Carbide - WC <Wt%=82.0 (4.2)>W2C <

11、Wt%=18.0 (0.9)>Tungsten Carbide=82.0%W2C=18.0%Wt%Quantitative Analysis from Profile-Fitted Peaks精品资料_LiCoO2 <Wt%=48.3 (4.1)>Silicon - Si <Wt%=51.7 (4.4)>LiCoO2=48.3%Wt%Silicon=51.7%Quantitative Analysis from Profile-Fitted Peaks具体 PDF 卡片结果：1.WCPDF#79-0743: QM=Calculated(C); d=Calculat

12、ed; I=CalculatedTungsten CarbideW2 CRadiation=CuKa1Lambda=1.54060 Filter=Calibration= 2T=18.769-89.599I/Ic(RIR)=10.80Ref: Calculated from ICSD using POWD-12+ (1997)Hexagonal - Powder Diffraction,P-31m (162)Z=3 mp=CELL: 5.19 x 5.19 x 4.724 <90.0 x 90.0 x 120.0> P.S=hP9 ($GE) (C5 W12)Density(c)=

13、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)精品资料_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 diff

14、raction 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-Thetad(?)I(f)( h k l)Theta 1/(2d)2pi/d n218.7694.72400.1(001)9.3840.10581.330119.7364.49470.1(100)9.8680.11121.397927.3663.25630.1(101)13.6830.15351.929634.5352

15、.595021.9(110)17.2670.19272.421338.0662.362023.6(002)19.0330.21172.660139.5922.2744100.0(-1-1 1)19.7960.21982.762543.2342.09090.1(102)21.6170.23913.005144.6132.02940.1(201)22.3060.24643.096152.3321.746815.0(-1-1 2)26.1660.28623.597156.4721.62810.1(202)28.2360.30713.859157.6121.59860.1(-2-1 1)28.8060

16、.31283.930461.8791.498216.2(300)30.9390.33374.193865.2811.42810.1(301)32.6410.35014.399669.8051.346215.2(-1-1 3)34.9030.37144.667372.8351.29752.0(220)36.4170.38544.842575.0111.265215.2(302)37.5050.39524.9663精品资料_75.9991.251211.5(-2-2 1)37.9990.39965.021979.4431.20530.1(311)39.7210.41485.212881.4191.

17、18102.1(004)40.7100.42345.320283.6701.15490.1(-2-1 3)41.8350.43305.440685.2721.13722.8(-2-2 2)42.6360.43975.525088.6431.10250.1(-3-1 2)44.3220.45355.699289.5991.09320.1(401)44.8000.45745.7477PDF#89-2727: QM=Calculated(C); d=Calculated; I=CalculatedTungsten CarbideW CRadiation=CuKa1Lambda=1.54060 Fil

18、ter=Calibration= 2T=31.509-84.081I/Ic(RIR)=15.71Ref: Calculated from ICSD using POWD-12+Hexagonal - Powder Diffraction,P-6m2 (187)Z=1 mp=CELL: 2.906 x 2.906 x 2.837 <90.0 x 90.0 x 120.0>P.S=hP2 (?)Density(c)=15.672Density(m)=15.13AMwt=195.86Vol=20.75F(9)=999.9(.0000,9/0)Ref: Parthe, E., Sadago

19、pan, 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 0.00/1精品资料_FIZ=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-undRoentgenb

20、eugungsuntersuchungenueberdieStrukturdesWolframcarbides W C und Vergleich mit aelteren Elektronenbeugungsdaten d a (P6-M2)NO2-Thetad(?)I(f)( h k l)Theta 1/(2d)2pi/d n231.5092.837044.0(001)15.7540.17622.214735.6452.5167100.0(100)17.8230.19872.496648.3021.882788.2(101)24.1510.26563.337464.0291.453017.

21、9(110)32.0140.34414.324365.7801.41855.4(002)32.8900.35254.429573.1131.293218.8(111)36.5570.38664.858475.4891.25839.0(200)37.7450.39744.993377.1211.235716.6(102)38.5600.40465.084684.0811.150313.9(201)42.0410.43475.46242. LiCoOSiPDF#75-0532: QM=Calculated(C); d=Calculated; I=Calculated精品资料_Lithium Cob

22、alt OxideLi Co O2Radiation=CuKa1Lambda=1.54060 Filter=Calibration=2T=18.930-87.020I/Ic(RIR)=4.38Ref: Calculated from ICSD using POWD-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>P.S=hR4 (?)Density(c)=5.049Density(m)=4.71AMwt=97.87Vol=9

23、6.54F(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 1.41/1 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

24、-x O System h ba (R3-MH) ABX22-Thetad(?)I(f)( h k l)Theta 1/(2d)2pi/d n218.9304.6840100.0(003)9.4650.10671.341437.3872.403328.8(101)18.6940.20802.614438.4042.34203.7(006)19.2020.21352.682839.0572.30439.2(012)19.5280.21702.7267精品资料_45.2192.003651.9(104)22.6090.24953.135949.4351.84217.7(015)24.7170.27

25、143.410859.1221.56131.0(009)29.5610.32024.024359.5971.55008.4(107)29.7980.32264.053665.4221.425410.4(018)32.7110.35084.408066.3171.408310.7(110)33.1590.35504.461569.6601.34876.7(113)34.8300.37074.658878.4871.21761.2(1010)39.2430.41065.160378.6831.21512.0(021)39.3420.41155.171179.3201.20691.8(116)39.

26、6600.41435.206179.7361.20170.9(202)39.8680.41615.228882.2641.17101.2(0012)41.1320.42705.365783.9111.15223.8(024)41.9550.43405.453485.7911.13172.1(0111)42.8960.44185.552287.0201.11880.8(205)43.5100.44695.6160PDF#89-2955: QM=Calculated(C); d=Calculated; I=CalculatedSiliconSiRadiation=CuKa1Lambda=1.540

27、60 Filter=Calibration=2T=28.445-88.041I/Ic(RIR)=4.55Ref: Calculated from ICSD using POWD-12+精品资料_Cubic - (Unknown),Fd-3m (227)Z=8 mp=CELL: 5.43029 x 5.43029 x 5.43029 <90.0 x 90.0 x 90.0>P.S=cF8 (?)Density(c)=2.330Density(m)=2.329Mwt=28.09Vol=160.13F(7)=999.9(.0000,7/0)Ref: Straumanis, M.E., B

28、orgeaud, 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 crystal bar: 5.43048 (Dm=2.3289).M Cell for powder, unheated: 5.43081.M Cell for powder, h

29、eated: 5.43070.M PDF 00-027-1402.No R value given.At least one TF missing.See PDF 01-075-0589.Perfectionof the latticeof dislocation-freesilicon,studiesby the lattice-constantanddensity method a (FD3-MS) N2-Thetad(?)I(f)( h k l)Theta 1/(2d)2pi/d n228.4453.1352100.0(111)14.2230.15952.0041347.3071.919

30、955.4(220)23.6540.26043.2727856.1281.637330.0(311)28.0640.30543.837611精品资料_58.8621.56760.1(222)29.4310.31904.00821269.1381.35766.9(400)34.5690.36834.62831676.3851.24589.5(331)38.1930.40145.04351988.0411.108511.5(422)44.0210.45115.668424六 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

31、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2d sinn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；精品资料_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。在线状焦点 S 到试样 O 和试样产生的衍射线到探测器的光路上还安装有多个光阑以限制 X 射线的发散；当探测器由低角到高角转动的过程中将逐一探测和记录各条衍射线的位置 （2角度）和强度。 探测器