X射线衍射实验报告Word格式文档下载.docx
《X射线衍射实验报告Word格式文档下载.docx》由会员分享,可在线阅读,更多相关《X射线衍射实验报告Word格式文档下载.docx(12页珍藏版)》请在冰豆网上搜索。
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。
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
10-80
8°
/min
40KV
250mA
7)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:
五实验数据处理
1物相鉴定结果
2定量分析结果
(1)WC
USER:
user
JADE:
QuantitativeAnalysisfromProfile-FittedPeaks
DATE:
Thursday,Jan01,200401:
16a
FILE:
[005WC.raw]
SCAN:
25.0/125.0/0.02/1(sec),Cu(40kV,250mA),I(max)=40668,10-28-1013:
19
PROC:
[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-$-epsilonW2C10.8017.162166.702861.018.0(0.9)18.0(0.9)16.7(1.1)10.072427(1893)6967(142)
2-ThetaFWHMHeightHeight%Area(a1)Area%I(r)I(p)I%-I(r)(hkl)
35.616(0.004)0.213(0.012)30158(1046)100.0479781(21469)100.0100.0100.00.0(100)
39.547(0.002)0.148(0.005)6967(142)100.072427(1894)100.0100.0100.00.0(-1-11)
(2)LiCoOSi
04a
[LiCoOSi(39).raw]
10.0/80.0/0.02/1(sec),Cu(40kV,250mA),I(max)=8718,08-27-1313:
27
Lithiumcobalt(III)oxideLiCoO24.385.049192.28970.848.3(4.1)48.3(4.1)30.1(3.2)10.044727(2619)5010(263)
SiliconSi4.552.32960.60141.151.7(4.4)51.7(4.4)69.9(7.5)10.049763(3069)6558(343)
18.897(0.005)0.144(0.007)5010(263)100.044727(2620)100.0100.0100.00.0(003)
28.409(0.005)0.131(0.006)6558(343)100.049763(3070)100.0100.0100.00.0(111)
3点阵常数精确测定结果
具体PDF卡片结果:
1.WC
PDF#79-0743:
QM=Calculated(C);
d=Calculated;
I=Calculated
TungstenCarbide
W2C
Radiation=CuKa1Lambda=1.54060Filter=
Calibration=2T=18.769-89.599I/Ic(RIR)=10.80
Ref:
CalculatedfromICSDusingPOWD-12++(1997)
Hexagonal-PowderDiffraction,P-31m(162)Z=3mp=
CELL:
5.19x5.19x4.724<
90.0x90.0x120.0>
P.S=hP9($GE)(C5W12)
Density(c)=17.162Density(m)=17.27AMwt=379.71Vol=110.20F(23)=999.9(.0000,32/0)
Epicier,T.,Dubois,J.,Esnouf,C.,Fantozzi,G.,Convert,P.
ActaMetall.,v36p1903(1988)
StrongLines:
2.27/X2.36/22.60/21.50/21.35/21.27/21.75/21.25/11.14/11.18/1
FIZ=065700:
ITFTEMMentioned.
NeutronpowderdiffractionstudiesoftransitionmetalhemicarbidesM2C1-x-II.
InsituhightemperaturestudyonW2C1-xandMo2C1-xkdcba(P3-1M)NO2
2-Thetad(?
)I(f)(hkl)Theta1/(2d)2pi/dn^2
18.7694.72400.1(001)9.3840.10581.3301
19.7364.49470.1(100)9.8680.11121.3979
27.3663.25630.1(101)13.6830.15351.9296
34.5352.595021.9(110)17.2670.19272.4213
38.0662.362023.6(002)19.0330.21172.6601
39.5922.2744100.0(-1-11)19.7960.21982.7625
43.2342.09090.1(102)21.6170.23913.0051
44.6132.02940.1(201)22.3060.24643.0961
52.3321.746815.0(-1-12)26.1660.28623.5971
56.4721.62810.1(202)28.2360.30713.8591
57.6121.59860.1(-2-11)28.8060.31283.9304
61.8791.498216.2(300)30.9390.33374.1938
65.2811.42810.1(301)32.6410.35014.3996
69.8051.346215.2(-1-13)34.9030.37144.6673
72.8351.29752.0(220)36.4170.38544.8425
75.0111.265215.2(302)37.5050.39524.9663
75.9991.251211.5(-2-21)37.9990.39965.0219
79.4431.20530.1(311)39.7210.41485.2128
81.4191.18102.1(004)40.7100.42345.3202
83.6701.15490.1(-2-13)41.8350.43305.4406
85.2721.13722.8(-2-22)42.6360.43975.5250
88.6431.10250.1(-3-12)44.3220.45355.6992
89.5991.09320.1(401)44.8000.45745.7477
PDF#89-2727:
WC
Calibration=2T=31.509-84.081I/Ic(RIR)=15.71
CalculatedfromICSDusingPOWD-12++
Hexagonal-PowderDiffraction,P-6m2(187)Z=1mp=
2.906x2.906x2.837<
P.S=hP2(?
)
Density(c)=15.672Density(m)=15.13AMwt=195.86Vol=20.75F(9)=999.9(.0000,9/0)
Parthe,E.,Sadagopan,V.
Monatsh.Chem.,v93p263(1962)
2.52/X1.88/92.84/41.29/21.45/21.24/21.15/11.26/11.42/10.00/1
FIZ=043380:
PDF00-025-1047.
MDescribedalsoasmineralfromMengyin,ShadongandDaSichuan,China.
AtleastoneTFimplausible.
ITFSeePDF01-072-0097.
Neutronen-undRoentgenbeugungsuntersuchungenueberdieStrukturdesWolframcarbidesWCundVergleichmitaelterenElektronenbeugungsdatenda(P6-M2)NO
31.5092.837044.0(001)15.7540.17622.2147
35.6452.5167100.0(100)17.8230.19872.4966
48.3021.882788.2(101)24.1510.26563.3374
64.0291.453017.9(110)32.0140.34414.3243
65.7801.41855.4(002)32.8900.35254.4295
73.1131.293218.8(111)36.5570.38664.8584
75.4891.25839.0(200)37.7450.39744.9933
77.1211.235716.6(102)38.5600.40465.0846
84.0811.150313.9(201)42.0410.43475.4624
2.LiCoOSi
PDF#75-0532:
LithiumCobaltOxide
LiCoO2
Calibration=2T=18.930-87.020I/Ic(RIR)=4.38
Rhombohedral-(Unknown),R-3m(166)Z=3mp=
2.8166x2.8166x14.052<
P.S=hR4(?
Density(c)=5.049Density(m)=4.71AMwt=97.87Vol=96.54F(19)=999.9(.0000,19/0)
Johnston,W.D.,Heikes,R.R.,Sestrich,D.
J.Phys.Chem.Solids,v7p1(1958)
4.68/X2.00/52.40/31.41/11.43/12.30/11.55/11.84/11.35/11.15/1
FIZ=029225:
AtleastoneTFmissing.
ThePreparation,Crystallography,andMagneticPropertiesoftheLixCo1-xOSystemhba(R3-MH)ABX2
18.9304.6840100.0(003)9.4650.10671.3414
37.3872.403328.8(101)18.6940.20802.6144
38.4042.34203.7(006)19.2020.21352.6828
39.0572.30439.2(012)19.5280.21702.7267
45.2192.003651.9(104)22.6090.24953.1359
49.4351.84217.7(015)24.7170.27143.4108
59.1221.56131.0(009)29.5610.32024.0243
59.5971.55008.4(107)29.7980.32264.0536
65.4221.425410.4(018)32.7110.35084.4080
66.3171.408310.7(110)33.1590.35504.4615
69.6601.34876.7(113)34.8300.37074.6588
78.4871.21761.2(1010)39.2430.41065.1603
78.6831.21512.0(021)39.3420.41155.1711
79.3201.20691.8(116)39.6600.41435.2061
79.7361.20170.9(202)39.8680.41615.2288
82.2641.17101.2(0012)41.1320.42705.3657
83.9111.15223.8(024)41.9550.43405.4534
85.7911.13172.1(0111)42.8960.44185.5522
87.0201.11880.8(205)43.5100.44695.6160
PDF#89-2955:
Silicon
Si
Calibration=2T=28.445-88.041I/Ic(RIR)=4.55
Cubic-(Unknown),Fd-3m(227)Z=8mp=
5.43029x5.43029x5.43029<
90.0x90.0x90.0>
P.S=cF8(?
Density(c)=2.330Density(m)=2.329Mwt=28.09Vol=160.13F(7)=999.9(.0000,7/0)
Straumanis,M.E.,Borgeaud,P.,James,W.J.
J.Appl.Phys.,v32p1382(1961)
3.14/X1.92/61.64/31.11/11.25/11.36/11.57/10.00/10.00/10.00/1
FIZ=043610:
MMeasuredatunetchedcrystalfragments.
MCellforetchedcrystalbar:
5.43048(Dm=2.3289).
MCellforpowder,unheated:
5.43081.
MCellforpowder,heated:
5.43070.
MPDF00-027-1402.
NoRvaluegiven.
AtleastoneTFmissing.
SeePDF01-075-0589.
Perfectionofthelatticeofdislocation-freesilicon,studiesbythelattice-constantanddensitymethoda(FD3-MS)N
28.4453.1352100.0(111)14.2230.15952.00413
47.3071.919955.4(220)23.6540.26043.27278
56.1281.637330.0(311)28.0640.30543.837611
58.8621.56760.1(222)29.4310.31904.008212
69.1381.35766.9(400)34.5690.36834.628316
76.3851.24589.5(331)38.1930.40145.043519
88.0411.108511.5(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θ与λ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(θ-2θ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2θ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