4 X射线衍射实验方法

1EE--mail:mail:[e-mail]@126.comTEL:022TEL:022--26582288265822882„DebyeScherrer1916„„„1Debye-scherrermethod„2focusingmethedX„3pinholemethodX„3„„X4„„„„„„„56„XX()X„XX„0.2-1.2mm„„X„7„114.6mm„„57.3mm180mm360º2º„114.6mm1º891011„„0.5mm„„250325103cm10-5cm„„„12„0.5mm10mm„1„2„323mm„413„„1X„14„2X„15„3X„16„1CrFeCoVMnFe2W18Cr4VFe-KaCrVCr3AlMgCuMoAl„K35X„17„2L2L’„RθRL43.572=θ2R57.3mmθ2L/22R114.6mmθ2L418„2θ90ºφ2R57.3mm2R114.6mm19„(1)—θ1-1'2-2'3-3'„(2)C0.1mm„(3)2Ll2L22L3„(4)θ„(5)d„(6)I/I1„(7)„(8)20aλaλθ2sin12sinθN222lkh++21„12345689…715232831…„24681012141618…123456789…„:3:4:8:11:12:16:19:20:24:…=l1.332.673.6745.336.336.08…221023„1λKaλKβθαθβ2KαKβ„KαKβ24„1715232831„2„qP100110110200110200P6110P12„3HKLHKLHKL25„„1X„2„d∆d∆Lϕ26„2L=R·4θ„dn2sinλθ=„ddn∆−=∆22cosλθθdd∆−=∆θθθsincos271R2θKα1Kα2283XX4X29XX303132332402.2.2PhilipsX34D8-DiscovreBruker199935X„.X„„X„„„36.X3738„X„1HOOC≤0.1mm„„392XXXTSSOO3SFABGSG(F)404BFGEOK5θXXθθ4142„143„21XSOF2(hkl)3)hkl==θ4)π-2θ5)44XSF3hklF454θsin2Rr=rRKπθSK=Rsin(90º-θ)=Rcosθr=SK/sin(π-2θ)=Rcosθ/sin2θ=R/2sinθθ=0∞θ=90º2r=R465„„„47„KβX„CuKα36%48„„X22cos12θ+22cos2cos122αθ⋅+49ab)0.08mm×10mmaXXX1.5ºbXFTaMo32mm0.05mm0.43mm50„X„XS1.5mm×10mm30º0.08mm×10mm„„„SS1(a)(b)S2S251„TaMo32mm0.05mm0.43mm„XX1.5º„aX„b2θ„1º3º4º.„F„52535455tkkkkKVAIFRIρµρ1∞1234IARρFµΙΑρV,K56X„X„1„2„3„457158„X„600900VX„„X103~105“”„XCR1„X59200Al600900X103105l0001500l0810960„„110-6s„2„3„4„5„„1„261„„X„„10-4s622„„11081091~10V„2X„X„3X„X„Cu-Ka)„4„6336465„X()0.5XX„„X10045814l06X()„10-5sX“”664XSi(Li)N=∆E/εNl001.33×10-4Pa67„1„2„3681„()X„()692„„„x—y„703„„()„()RC„RC(I2θ)71RCSacCbcRMRCRCRCRC72„„1„2()„731„.„„+.„2θ0º5º~6º2θ2θ„4min2θ20º-100º20min„742()„„2θ(0.02)(5s)2θ()„2θ7520304050607080θα-Fe(Nb)θθµFe-NbµµµµµξξρξSmHyξξξSm2Fe16.5Nb0.5byHDDRtreatmentat8000Cbutshortofvacuum-pumping2θ(degree)ξρSm2(Fe,Nb)17ρIntensity(arb.u.)76„1„XHCG„130º1l2º16º14º12º1º4º„130º112º16º14º12º1º4º„0.05mm0.1mm0.2mm0.4mm2.0mm772A3X7831º-4º/min(º)/min79XRD„DiffracATqualitativeprogrameditorV3.20„Measurementrangeeditionmenu„Rangelabel:1Delaytostart:0.0s„Stepdrive:Normal,coupledStepmode:Stepscan„StepTime:1.0sRangetime:52mn1s„Stepsize:0.020„2thetaSample„Startposition20.00010.000L„Stopposition80.00040.000„Divergenceslit:xxxxx?Antiscatterslit:xxxxx?Detectorslit:OUT„Oscillation:Amplitude:Speed:„Rotation:None„Temperature:RoomSlewingspeed:xx.xxC/s„Nextrange:Iteration:noneNesting:„Tubecurrent:50mATubevoltage:35kV„Meas.channel:1Detectorvoltage:850VAmplifier:2„Baselevel:0.800VUpperlevel:2.300VAdjustment:Automatic„xscale:0.00?/cmyscale:1000.Cps/cm„Alabelisrequirediftherangeisreferencedelsewhereintheprogram„80XRD81„„„82„*„*„**„CuKαλ1.54056α=4.04942θ***„CuKαλ1.540560.02%α=0.2861nm2θ8***„CuKαλ1.540562θ=27.4531.845.654.0556.766.573.375.684.3*****83„X**„**„**„*„Si(Li)*„θθθ2θ**„***