X射線衍射實(shí)驗(yàn)報(bào)告

1、_中南大學(xué)X 射線衍射實(shí)驗(yàn)報(bào)告材料科學(xué)與工程 學(xué)院材料國(guó)際專業(yè)1401班級(jí)姓名蔡云偉學(xué)號(hào)0605140118同組者實(shí)驗(yàn)日期2016 年05 月18日指導(dǎo)教師黃繼武評(píng)分分評(píng)閱人評(píng)閱日期一、實(shí)驗(yàn)?zāi)康?) 掌握 X 射線衍射儀的工作原理、操作方法；2) 掌握 X 射線衍射實(shí)驗(yàn)的樣品制備方法；3) 學(xué)會(huì) X 射線衍射實(shí)驗(yàn)方法、實(shí)驗(yàn)參數(shù)設(shè)置，獨(dú)立完成一個(gè)衍射實(shí)驗(yàn)測(cè)試；4) 學(xué)會(huì) MDI Jade 6 的基本操作方法；5) 學(xué)會(huì)物相定性分析的原理和利用 Jade 進(jìn)行物相鑒定的方法；6) 學(xué)會(huì)物相定量分析的原理和利用 Jade 進(jìn)行物相定量的方法。本實(shí)驗(yàn)由衍射儀操作、物相定性分析、物相定量分析三個(gè)獨(dú)立的實(shí)

2、驗(yàn)組成，實(shí)驗(yàn)報(bào)告包含以上三個(gè)實(shí)驗(yàn)內(nèi)容。二、實(shí)驗(yàn)原理精品資料_根據(jù)布拉格定律， 我們可以知道， 只有在特殊的入射角度時(shí)我們才能得到衍射圖像。所以，根據(jù)這一原理，我們?cè)谑褂昧税裍 射線和探測(cè)器放在環(huán)形導(dǎo)軌上的方法，把每個(gè)方向的結(jié)果都探測(cè)一遍，最終收集到能發(fā)生衍射的衍射峰。根據(jù)結(jié)果，推算晶面，判斷晶體構(gòu)型，判斷元素種類。三、儀器與材料1) 儀器： 18KW 轉(zhuǎn)靶 X 射線衍射儀2)數(shù)據(jù)處理軟件：數(shù)據(jù)采集與處理終端與數(shù)據(jù)分析軟件MDI Jade 63) 實(shí)驗(yàn)材料： WC( 碳化鎢 )、LiCoOSi四、實(shí)驗(yàn)步驟1 測(cè)量數(shù)據(jù)1) 準(zhǔn)備樣品；2) 打開(kāi) X 射線衍射儀；精品資料_3) 按下“Door ”按

3、鈕，聽(tīng)到報(bào)警；4) 向右拉開(kāi)“常規(guī)衍射儀門”，裝好樣品；5) 向左輕拉“常規(guī)衍射儀門”，使之合上；6) 打開(kāi)“控制測(cè)量”程序，輸入實(shí)驗(yàn)條件和樣品名，開(kāi)始測(cè)量；表 1 實(shí)驗(yàn)參數(shù)設(shè)定：儀器掃描范圍掃描度電壓電流D/max 2500 型 X 射線衍射儀10-808°/min40KV250mA7) 按相同的實(shí)驗(yàn)條件測(cè)量其它樣品的衍射數(shù)據(jù)。2 物相鑒定1) 打開(kāi) Jade ，讀入衍射數(shù)據(jù)文件；2) 鼠標(biāo)右鍵點(diǎn)擊 S/M 工具按鈕，進(jìn)入“Search/Match ”對(duì)話界面 ;3) 選擇“Chemistry filter ，”進(jìn)入元素限定對(duì)話框，選中樣品中的元素名稱，然后點(diǎn)擊 OK 返回對(duì)話框，

4、再點(diǎn)擊 OK ；4) 從物相匹配表中選中樣品中存在的物相。在所選定的物相名稱上雙擊鼠標(biāo)，顯示 PDF 卡片，按下 Save 按鈕，保存 PDF 卡片數(shù)據(jù)；5) 在主要相鑒定完成后，對(duì)剩余未鑒定的衍射峰涂峰，做“ Search/Match ”，直至全部物相鑒定出來(lái)。6) 鼠標(biāo)右鍵點(diǎn)擊“打印機(jī)”圖標(biāo)，顯示打印結(jié)果，按下“Save ”按鈕，輸出物相鑒定結(jié)果。7) 以同樣的方法標(biāo)定其它樣品的物相 ,物相鑒定實(shí)驗(yàn)完成。精品資料_3 物相定量分析1) 在 Jade 窗口中，打開(kāi)一個(gè)多相樣品的衍射譜；2)完成多相樣品的物相鑒定，物相鑒定時(shí)，選擇有RIR 值的 PDF 卡片；3) 選擇每個(gè)物相的主要未重疊的衍

5、射峰進(jìn)行擬合，求出衍射峰面積；4) 選擇菜單“Options|Easy Quantitative ”，按絕熱法計(jì)算樣品中兩相的重量百分?jǐn)?shù)；5) 按下“Save ”按鈕，保存定量分析結(jié)果，定量分析數(shù)據(jù)處理完成。計(jì)算公式 :aKK baRIRaI aAl 2O 3, WabRIRbaAl 2O 3(I aIb Kb )五 實(shí)驗(yàn)數(shù)據(jù)處理1 物相鑒定結(jié)果精品資料_2 定量分析結(jié)果（1）WC USER: userJADE: Quantitative Analysis from Profile-Fitted Peaks精品資料_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%精品資料_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)精品資料_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 點(diǎn)陣常數(shù)精確測(cè)定結(jié)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精品資料_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具體 PDF 卡片結(jié)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)精品資料_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精品資料_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精品資料_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精品資料_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精品資料_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+精品資料_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精品資料_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 結(jié)果與討論一、實(shí)驗(yàn)原理本次實(shí)驗(yàn)采用的儀器為X 射線衍射儀，它是按照晶體對(duì)X 射線衍射的幾何原理設(shè)計(jì)制造的。布拉格方程是 X

31、射線衍射儀最基本的理論基礎(chǔ)，也是進(jìn)行X 射線檢測(cè)最根本和重要的理論依據(jù)之一。由2d sinn知，確定了一組相互對(duì)應(yīng)的與便可求出一組干涉面的面間距d，當(dāng)干涉指數(shù)互質(zhì)時(shí)， 干涉面就代表一族真實(shí)的晶面。因?yàn)榇嬖谙到y(tǒng)消光，并非所有滿足布拉格方程的干涉面都有對(duì)應(yīng)的衍射條紋。為保證能得到足夠的衍射譜線以分析，X 射線衍射儀使用的是粉末樣品，用單色（標(biāo)識(shí)） X 射線照射多晶體試樣，即多晶體衍射方法，并且同時(shí)使樣品轉(zhuǎn)動(dòng)（-2 連動(dòng)），設(shè)計(jì) 2:1 的角速度比，目的是確保探測(cè)的衍射線與入射線始終保持 2的關(guān)系，即入射線與衍射線以試樣表面法線為對(duì)稱軸，在兩側(cè)對(duì)稱分布；精品資料_輻射探測(cè)器接收到的衍射是那些與試樣表面平行的晶面產(chǎn)生的衍射；同樣的晶面若不平行于試樣表面，即使產(chǎn)生衍射，其衍射線進(jìn)不了探測(cè)器，不能被接受；X射線源由X 射線發(fā)生器產(chǎn)生，其線狀焦點(diǎn)位于測(cè)角儀周圍位置上固定不動(dòng)。在線狀焦點(diǎn) S 到試樣 O 和試樣產(chǎn)生的衍射線到探測(cè)器的光路上還安裝有多個(gè)光闌以限制 X 射線的發(fā)散；當(dāng)探測(cè)器由低角到高角轉(zhuǎn)動(dòng)的過(guò)程中將逐一探測(cè)和記錄各條衍射線的位置 （2角度）和強(qiáng)度。 探測(cè)器