XRD-Rietveld法用于水泥基材料物相的定量分析-李华

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ConcreteAbstract:XRD-RietveldmethodhasbeenadoptedforquantitativeanalysisofphasesincementpowderandphasesinmixedsamplesofcementandpurecalciumhydroxidebasedontheTOPASsoftwaretheRietveldanalysisvalueswerecomparedwiththermalanalysisval-uesandtheactualpreparationvalues.TheresultsshowedthatRietveldanalysisvaluesshowedgoodagreementwiththeactualpreparationvaluesofmixedsamplesandtheaccuracydegreeofRietveldmethodwasatleastaswellasthatofTG/DSCmethodwhichwascommonlyusedinquantitativeanalysisofcalciumhydroxide.ByaddingappropriateinternalstandardsubstanceXRD-Rietveldmethodcouldbeef-fectivelyuseinquantitativeanalysisofsulfateattackproductsincement-basedmaterials.Thisworkhaspracticalsignificanceonthestudyofsulfateattackofcement-basedmaterial.Keywords:XRDRietveldmethodcement-basedmaterialphasequantitativeanalysisQuantitativeanalysisofphasesforcement-basedmaterialsbyXRD-RietveldmethodLIHua1SUNWei2LIUJia-ping11.StateKeyLaboratoryofHighPerformanceCivilEngineeringMaterialsJiangsuAcademyofBuildingScienceCo.Ltd.Nanjing211103China2.CollegeofMaterialsScienceandEngineeringSoutheastUniversityNanjing211189ChinaXRD-RietveldTOPAS-Rietveld。RietveldRi-etveldTG/DSCXRD-Rietveld。XRDRietveldTU528.01A1002-3550201301-0001-051211.2111032.211189XRD-Rietvelddoi10.3969/j.issn.1002-3550.2013.01.00120131279Number1in2013TotalNo.2792012-07-039732009CB62320351078186BK2010071THEORETICALRESEARCH0[1]。、、。X、、Khklhkl、、。RietveldX。[1]。Rietveld。[2-3]。X-Rietveld。-。1Rietveld[4-5]X1··、。RietveldSj=KVjVju2=KmjZjMjVju1wj=mjpΣmp=SjZjMjVjupΣSpZpMpVpu2S———V———Vu———Z———“”“”M———m———w———。。Z、M、VuS2。SM=ΣwiYoi-Yci23Yoi———Yci———wi———1/Yoi。M。Yci=Ybi+jΣSjjkΣLjk|Fjk|2Φ2θji-2θjkPjkAj4Ybi———Sj———jk———hklLk———、Fk———Φ———2θ———Pk———Aj———j。4SFkLkYciYoiS。R。R。RwpRwpRwp0。Rwp15%10%。SS1.0~2.0。22.1P·I52.5。P·I52.580μm9∶1、8∶27∶390C+10P、80C+20P、70C+30P。0.5~1h。5.0%Na2SO4Φ14mm×250mm0.35。Φ14mm×10mm50℃2d80μm。80μmα-Al2O31∶91h。。2.2LynxEyeBruker-AxsD8DISCOVERXCu40kV30mA4.0°stepsize=0.02°2θ0.30s/step7°~80°2θ。。33。3Rietveld3.1Rietveld100%。。[6]wj=wsSjZjMjVjuSsZsMsVsuwamorphous=1-Σwj-wswj′=wj1-wswamorphous′=wamorphous1-ws———jwamorphous———2··wj′———jwamorphous′———。XRD2θ=25°~35°“”C-S-H。。、α-Al2O3。3.2TOPASRietveldXRD-Rietveld1XRDRietveldTOPASXRD.raw、、、。Rwp。α-Al2O3XRDStructures/Quantitativeα-Al2O3。XRDChebyshevRXRD001March-DollaseR2。。44.1RietveldXRD-Rietveld。3XRD-Rietveld331。C3S、C2S、C3A、C4AF3/4、、、、。P·I。CaOH20.90%。。4.2-XRD-Rietveld-1XRD-Rietveld/%1.560.480.900.590.471.03MgOCaSO4CaOH2CaCO3SiO2CaSO4·0.5H2OC3SC2SC3AC4AFCaSO4·2H2OCaOK2SO4/%62.7614.193.4813.640.210.170.503··XRD-RietveldTG/DSC。XRD-Rietveld2Rwp6~10S1.1~1.4。23XRDRietveld0.21、1.340.78。XRD-RietveldTG/DSC43。43XRD-Rietveld0.50%1%5%RietveldTG/DSC。XRD-Rietveld。4.3。[7-11]XK、/BSE/IATG/DSC、、。5TG/DSC。DSC480~110℃、120~150℃、400~450℃、650~730℃4、、[11-12]。DSC30~170℃C-S-H[13]。、C-S-HTG/DSC。2-XRD-RietveldXRD90C+10P①80C+20P70C+30P0.211.340.78/%10.6310.5110.1421.3018.4721.3431.6029.9829.92/%10.4320.3730.50①CCementPPortlandite。/%10.0020.0030.003-XRD/%TG/DSC/%XRD/%TG/DSC/%90C+10P80C+20P70C+30P10.4320.3730.50①9.6219.6529.8710.7719.9029.85②9.9619.1829.220.380.350.133.801.750.430.404.102.600.040.820.78①、②=-0.90%。XRD-Rietveld64。Rietveld。4C3A0.61%4··3.06%8.76%5.40%。4Rwp=5.45S=1.47。5XRD-Rietveld。Rietveld-RietveldTG/DSCRietveld。XRD-Rietveld。[1].X[J].1996113407-414.[2]WALENTAGF譈LLMANNTGIMENEZM.QuantitativeRietveldanalysisofcementandclinker[J].Int.Cem.Rev.200151-54.[3]WESTPHALTWALENTAGF譈LLMANNTetal.Characterizsa-tionofcementitiousmaterials-PartIII[J].Int.Cem.Rev.200247-51.[4].X[M].2008262-274.[5]YOUNGRA.Therietveldmethod[M].OxfordUniversityPress1993.[6].X[M].2008287-288.[7].XK[J].2001334-38.[8].X[J].2003203334-337.[9]DIAMONDS.Themicrostructureofcementpasteandconcrete-avisualprimer[J].CementandConcreteComposites200426919-933.[10]SCRIVENERKL.Backscatteredelectronimagingofcementitiousmicrostructuresunder-standingandquantification[J].CementandConcreteComposites200426935-945.[11].[J].1997544-47.[12].[J].200728123-25.[13].[J].2009326-2953.1987-,,。59211103136551617564XRD-RietveldC2SC3AC4AFMgOSiO2K2SO4CaSO4·2H2OCaSO4·0.5H2OCaCO3CaOH2K2Ca2SO43K3NaSO42C3AH6C3SAl2O3*Na2SO4C6S3HC2SHC3S3H/%1.7430.6095.9980.2700.7280.5318.7581.1805.9753.05745.1880.5180.4295.3961.2081.27801.2864.1275.8115.9111.5690.5485.3980.2430.6550.4787.8821.0625.3772.75140.6690.4660.3864.8561.0871.15010.0001.1573.7145.2305.320*。!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!《2013》《》。、。《》、、、、、、。、。《》、“”。。《》65··

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