同步辐射小角和广角X射线散射在高分子材料研究中的应用

©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(50973103);973(2010CB934504);(YZ200927);(018);X15;:(1985-),,,,,E2mail:[e-mail];3:E2mail:[e-mail].X1,1,1,2,2,13(11,230029;21,,201204):X,,,X,X,:X;;21111[1],,,,:(1),;(2),,1:1[2]Figure1Aschematicofthethird2generationsynchrotronradiation(SR)lightsource[2]110©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:(1)X,,,(2);(2),100%;(3)X,,;(4)X;(5)X,,,,,,,,,,,,,,BrookhavenNSLSDaresburySRS(NSRL),,,,X,11,,(SSRF),2[2]Figure2Thebrillianceofdifferentgenerationlightsources112,,X(SAXSWAXS)X2201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.()()()(:),,,;(),,;;X,0111000nm,,X[3],X,ESRF123,56;NSLSDiamondEXXONMOBILENSLS,,,X,3[]Figure3PhotographofShanghaiSynchrotronRadiationFacility(SSRF)[],(),23,14,,310©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.[4]7,X(BL16B1)X,::520keV(V2MoK);:E/E61010-4@10keV:1011phs/s@10keV:014mm(h.)015mm(v.)@10keV:100ms:4Figure4DiagramofSSRFsmallangleX2rayscatteringbeamlineandstation,,Mar165CCD,,,,,;;1Table1ExperimentalconditionofSSRFsmallangleX2rayscatteringbeamlineandstation(1)(2)Linkam(1)CCD:Mar165CCD(2)1D(3)1D2m3m5m1120nm(=01124nm)4201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:(1)X,(300nm);(2),(),,;(3),,X,;(4),,,,;(5)X,2,,,X,,,,,,X5ALinkamTHM600(),011,30/min,X,XX(Kapton)XX,,5BLinkamCSS450(),450,LinkamTHM600,,,X,,Kapton,,6,,1000%,0158m/s580m/s,510©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(),,,7B(),6201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.[5][6](iPP),SAXS/WAXS8Ryan,=01103nm,SAXS8m,WAXS(MSGC),SAXS/WAXSiPP(8mm,1mm)DSC,LinkamDSC20/min180,5min,50/minT1LinkamDSCSAXS/WAXS,X8s,10sSAXSq,WAXSHDPE,WAXS2710©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(=01154nm)8BM26BDUBBLE(ESRF)SAXS/WAXSFigure8SAXS/WAXSexperimentallayoutonBM26BDubblebeamlineattheESRF,France9iPP130SAXS/WAXS,SAXSq2I(q,t)WAXSI(2,t)I(q,t)qm,SAXSL=2/qmLp9,130Lp=19nmiPPSAXSWAXS,SAXSQsWAXS,SAXSQs:Qs=0q2I(q,t)dqq2q1q2I(q,t)dq(1)q,q1q2,q9iPP130SAXS/WAXS[2WAXSCuK(=01154nm))]Figure9SAXS/WAXSdevelopmentduringisothermalcrystallizationofiPPat130.TheWAXSdataarepresentedin2renormalizedtoCuK(=01154nm)WAXSPearson,iPP,10WAXS,,,WAXS,(110)(040)11iPPSAXSQ,(8201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.)10WAXSPearsonFigure10FittingofWAXSdatausingaPearsonVIIfunctionfortheBraggpeakssuperimposedonapolynomialbackground11iPP(SAXSQ)Figure11IsothermalcrystallizationofiPPatseveraltemperaturesshownbythedevelopmentoftheinvariantQ,calculatedfromtheSAXSdata12iPP130SAXSWAXS,Avrami,Avrami:1-Xs=e-Ktn(2)K,Xs,Xs=Ws(t)/Xw()(SAXS),nAvrami,12,n=314,,Avrami,n,,SAXSWAXS,,,,,SAXSWAXS,SAXSWAXS,13,SAXS500s,,WAXS1000sSAXS,WAXS,,Ryan,Cahn2Hilliard,,SAXS/WAXS,SAXSWAXS,910©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.()Figure13SAXS/WAXSdataofisothermalcrystallizationforiPPat140,TheinsertshowsSAXS/WAXSdataintheearlystageofcrystallization,,:(1)X,,X;(2),X,SAXSWAXS312X[79],,,,,,,,Leibler1980Macromolecules,Macromolecules,14,XX,X,01201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(2b2)Xq1234,,,q13273,1232,14[10]Figure14Self2assembledorderednanostructureofdiblockcopolymer[10]15PEO2b2PBhXFigure15SmallX2rayscatteringcurveofPEO2b2PBhdiblockcopolymer,,,,,,SAXSWAXS,16PEO2b2PSSAXSWAXSWAXS,SAXSSAXSWAXS,,,,,1110©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(a)WASX(b)Figure161DSAXS(a)andWAXS(b)patternsofPEO2b2PSduringcrystallization17(a)PEO2b2PSSAXS;(b)48SAXSFigure17(a)1DSAXSpatternsofPEO2b2PScrystallizedatdifferenttemperatures;(b)2DSAXSpatternofPEO2b2PScrystallizedat4917(a)X,,q32,,,17(b),perforated,,,,perforated,,PCL2b2PEO,18PCL2b2PEOSAXSWAXSPCL,,WAXS,PCL,PEO15,PEO,WAXSPEO,PEOSAXSSAXSWAXS,PCL,PEO,[18(c)],PCL,,PEO,,PLLA()PDLA(),1/121201010©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(a)WAXS(b),cSAXSWAXSFigure181DSAXS(a)andWAXS(b)patternsduringstepwisecoolingofhighlyasymmetricPCL2b2PEOdiblockcopolymer,(c)EvolutionmodelofthemorphologyrevealedfromSAXS/WAXSpatternsduringstepwisecooling(),50,,:PLLA,PDLA,()PLLAPDLA,,19(PLLA2b2PDLA)WAXS,LD80/20[19(a)],145LD50/50,[19(