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MDIJade6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、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。2三、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MDIJade63)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/max2500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“Chemistryfilter”，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。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|EasyQuantitative”，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:3babOAlaOAlabRIRRIRKKK3232,)(abbaaaKIIIW五实验数据处理1物相鉴定结果42定量分析结果（1）WCUSER:userJADE:QuantitativeAnalysisfromProfile-FittedPeaksDATE:Thursday,Jan01,200401:16aFILE:[005WC.raw]SCAN:25.0/125.0/0.02/1(sec),Cu(40kV,250mA),I(max)=40668,10-28-1013:19PROC:[NewQuantitativeAnalysis]PhaseID(2)ChemicalFormulaRIRDxMACLACWt%Wt(n)%Vol(n)%#LI%-I(r){Area}{Height}TungstenCarbideWC15.7115.672161.732534.782.0(4.2)82.0(4.2)83.3(5.7)10.0479781(21469)30158(1046)Tungstencarbide-$-epsilonW2C10.8017.162166.702861.018.0(0.9)18.0(0.9)16.7(1.1)10.072427(1893)6967(142)2-ThetaFWHMHeightHeight%Area(a1)Area%I(r)I(p)I%-I(r)(hkl)35.616(0.004)0.213(0.012)30158(1046)100.0479781(21469)100.0100.0100.00.0(100)2-ThetaFWHMHeightHeight%Area(a1)Area%I(r)I(p)I%-I(r)(hkl)39.547(0.002)0.148(0.005)6967(142)100.072427(1894)100.0100.0100.00.0(-1-11)（2）LiCoOSiUSER:userJADE:QuantitativeAnalysisfromProfile-FittedPeaksDATE:Thursday,Jan01,200401:04aFILE:[LiCoOSi(39).raw]SCAN:10.0/80.0/0.02/1(sec),Cu(40kV,250mA),I(max)=8718,08-27-1313:27PROC:[NewQuantitativeAnalysis]PhaseID(2)ChemicalFormulaRIRDxMACLACWt%Wt(n)%Vol(n)%#LI%-I(r){Area}{Height}Lithiumcobalt(III)oxideLiCoO24.385.049192.28970.848.3(4.1)48.3(4.1)30.1(3.2)10.044727(2619)55010(263)SiliconSi4.552.32960.60141.151.7(4.4)51.7(4.4)69.9(7.5)10.049763(3069)6558(343)2-ThetaFWHMHeightHeight%Area(a1)Area%I(r)I(p)I%-I(r)(hkl)18.897(0.005)0.144(0.007)5010(263)100.044727(2620)100.0100.0100.00.0(003)2-ThetaFWHMHeightHeight%Area(a1)Area%I(r)I(p)I%-I(r)(hkl)28.409(0.005)0.131(0.006)6558(343)100.049763(3070)100.0100.0100.00.0(111)3点阵常数精确测定结果TungstenCarbide=82.0%W2C=18.0%Wt%TungstenCarbide-WCWt%=82.0(4.2)W2CWt%=18.0(0.9)QuantitativeAnalysisfromProfile-FittedPeaksLiCoO2=48.3%Silicon=51.7%Wt%LiCoO2Wt%=48.3(4.1)Silicon-SiWt%=51.7(4.4)QuantitativeAnalysisfromProfile-FittedPeaks6具体PDF卡片结果：1.WCPDF#79-0743:QM=Calculated(C);d=Calculated;I=CalculatedTungstenCarbideW2CRadiation=CuKa1Lambda=1.54060Filter=Calibration=2T=18.769-89.599I/Ic(RIR)=10.80Ref:CalculatedfromICSDusingPOWD-12++(1997)Hexagonal-PowderDiffraction,P-31m(162)Z=3mp=CELL:5.19x5.19x4.72490.0x90.0x120.0P.S=hP9($GE)(C5W12)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.ActaMetall.,v36p1903(1988)StrongLines:2.27/X2.36/22.60/21.50/21.35/21.27/21.75/21.25/11.14/11.18/1FIZ=065700:ITFTEMMentioned.NeutronpowderdiffractionstudiesoftransitionmetalhemicarbidesM2C1-x-II.InsituhightemperaturestudyonW2C1-xandMo2C1-xkdcba(P3-1M)NO22-Thetad(?)I(f)(hkl)Theta1/(2d)2pi/dn^218.7694.72400.1(001)9.3840.10581.330119.7364.49470.1(100)9.8680.11121.397927.3663.25630.1(101)13.6830.15351.929634.5352.595021.9(110)17.2670.19272.421338.0662.362023.6(002)19.0330.21172.660139.5922.2744100.0(-1-11)19.7960.21982.762543.2342.09090.1(102)21.6170.23913.005144.6132.02940.1(201)22.3060.24643.096152.3321.746815.0(-1-12)26.1660.28623.597156.4721.62810.1(202)28.2360.30713.859157.6121.59860.1(-2-11)28.8060.31283.930461.8791.498216.2(300)30.9390.33374.193865.2811.42810.1(301)32.6410.35014.399669.8051.346215.2(-1-13)34.9030.37144.667372.8351.29752.0(220)36.4170.38544.842575.0111.265215.2(302)37.5050.39524.966375.9991.251211.5(-2-21)37.9990.39965.021979.4431.20530.1(311)39.7210.41485.212881.4191.18102.1(004)40.7100.42345.320283.6701.15490.1(-2-13)41.8350.43305.4406785.2721.13722.8(-2-22)42.6360.43975.525088.6431.10250.1(-3-12)44.3220.45355.699289.5991.09320.1(401)44.8000.45745.7477PDF#89-2727:QM=Calculated(C);d=Calculated;I=CalculatedTungstenCarbideWCRadiation=CuKa1Lambda=1.54060Filter=Calibration=2T=31.509-84.081I/Ic(RIR)=15.71Ref:CalculatedfromICSDusingPOWD-12++Hexagonal-PowderDiffraction,P-6m2(187)Z=1mp=CELL:2.906x2.906x2.83790.0x90.0x120.0P.S=hP2(?)Density(c)=15.672Density(m)=15.13AMwt=195.86Vol=20.75F(9)=999.9(.0000,9/0)Ref:Parthe,E.,Sadagopan,V