材料研究方法综述

1Al2O3MgOSiO2OptionalratioheatingRawmaterialsingleelementmaterialAl:Aluminum(Cubic)Mg:Magnesium(Cubic)Mg:Magnesium(Hexagonal)Si:Silicon(Cubic)Si:Silicon(Hexagonal)Si:Silicon(Monoclinic)2Al-oxidesAl2O3CorundumAl2O3RubyAl2O3CubictypeAl2O3HexagonaltypeAl2O3TetragonaltypeAl2O3Orthohombictype…About30typesMg-oxidesMgOPericlase(Cubic)MgO(Cubic)MgO2(unknown)MgO4(Tetragonal)4types3Mg-Al-oxidesMgAl2O4SpinelMg-Al-OMgAl26O40Mg0.866Al1.830O3.611Mg0.388Al2.408O4Mg0.36Al2.44O4Crawfordite(Mg0.4Al0.6)Al1.8O4……Al-Si-oxidesAl2SiO5sillimaniteAl2SiO5kyaniteAl2SiO5andalusiteAl2SiO5sillimanite……4Al-Si-oxidesAl2SiO5sillimaniteAl2SiO5kyaniteAl2SiO5andalusiteAl2SiO5sillimanite……5Mg-Al-Si-oxidesMg2Al4Si5O18CordieriteMg3Al2Si3O12PyropeMg2(Al4Si5O18)CordieriteMg4Al10Si2O23sappirineMg2Al4Si5O18indialiteMg2Al3(Si3Al)O10O8chlorite…About50kindsTotally300-400typesofphase6Purpos：Todetermine(1)thechemicalcomposition,(2)thestructure,(3)thesurfacemorphology,(4)thephysicalandchemicalpropertiesofthematerials.71.Outline1.1Chemicalcompositionanalysis:todeterminethekindsandthecontentsoftheelementsinamaterial.QualitativeandQuantitative8QualitativeandQuantitativeQualitativeanalysisisusedtodeterminethekindsofcationsandanionsinasamplesubstanceQuantitativeanalysisisusedtodeterminethekindsandthecontentsofcationsandanionsinasamplesubstance9Describingthechemicalcomposition:Weightconcentration:forsolid,liquidGeneralelement%wtMicroElement:ug/g(g/t)(ppm)10-6Super-micro:ng/g(ppb)10-9HintElement:pg/g(ppt)10-12Volumeconcentration:forliquid,gasGeneral:mol/LMicro:mmol/L10ExpressingtheChemicalCompositiona)Formetal,singleelementmaterial,sulfide,andsomeothermaterialsthattheirionsarenotoxygen.ExpressingasElementcontent.Iron(钢材):Fe:99.00%wt,C:1.00%wtPyrrhotite(磁黄铁矿)(Fe1-xS):Fe:63.00%wtS:36.00%wtNi:0.50%wt11ExpressingtheChemicalCompositionb)Foroxide(氧化物),Silicate(硅酸盐),andsomeothermaterialsthattheirionisoxygen(carbonate碳酸盐,sulfate硫酸盐…).Whenexpressingtheircompositions,generallyasoxidetypes12Forexample:Orthoclass钾长石(KAlSi3O8):K2O15.13%wtSiO263.51%wtAl2O318.99%wtNa2O1.34%wtCaO0.13%wtFe2O30.09%wtCalcite方解石(CaCO3):CaO55.03%wtFeO0.12%wtMgO0.22%wtCO243.97%wt13有效位数及小数的进位取舍35.0145…当小数后2个有效位时等于:35.013个有效位时等于:35.0144舍6入,5单双(奇进偶不进)如：小数后取两位：35.045---35.0435.035---35.0435.0451---35.05141.2structuralAnalysis:Todeterminethearrangementoftheelementsinamaterial(确定物质中元素的排列组合方式)Crystalsystem(晶系)Cellparameters(晶胞参数)atomcoordinatesintheunitcell(原子坐标)andalsotodeterminethemineralphase(s)(物相分析)15Forexample:C(Carbon):canbegraphite(石墨)orbediamond,becausetheyhavedifferentstructure(atomarrangementisdifferent)SiO2：αQuartz,βquartz,……Al2[SiO4]O:Andalusite(红柱石)Kyanite(蓝晶石)16Describingthestructure:Crystalsystem:cubic,tetragonal,orthorhombic,monoclinic,triclinic,hexagonal,triogonal,Symmetry:plane(m),Center(c),Axles(1,2,3,4,6,3-,6-),CellParameters:a,b,c,α,β，AtomiccoordinatesForexample：halite(NaCl):Fm3ma=5.628ACl:4a,0,0,0Na:4b,½,½,½.171.3Morphologicalproperties(Surfaceobservation)MorphologicalpropertiesincludeMacro,Micro,SuperMicroproperties.Macro-bynakedeyes.Micro-bymicroscope,electronmicroscope…SuperMicro-ScanningtunnelingmicroscopyAtomicforcemicroscopy18Toobservetheshapeoftheparticles,theirboundarycharacteristic,insomecases,toobserveatomarrangementdirectly.(观察颗粒的形状、边界特征，有时甚至可以直接观察到原子级别)Generally,themorphologicalanalysisiscombinedwithchemicalanalysis.Itiscalledmicro-regionanalysis(bothchemicalandmorphologicalanalysis)(一般地，形貌分析和成分分析联合进行，此即所谓的微区分析－－既分析微形貌，有分析微区成分)191.4AnalysisofphysicalandchemicalpropertiesIncludingThermal,Light,electricity,mechanics,etc.202.AnalyzingMethods212.1ChemicalComposition2.1.1WetChemicalAnalysis:湿法化学分析solid,liquid,gasliquidchemicalreactioncalculatingchemicalanalyzingresult22Silicateanalysis(includingoxides)usedformostofthematerial:(称之为常规13项分析)SiO2,Al2O3,MgO,FeO,Fe2O3,CaO,K2O,Na2O,MnO,TiO2,P2O5,(H2O)+,(H2O)-percent(%wt),Bulksample(2.0g),longperiod(2weeks)Generally2validatingdigitsafterpoint.232.1.2Adsorptionspectroscope(Instrumentanalysis)Generalconcentration(%wt)tomicro(ug/g)andalsotohintconcentration(ng/g)solid,liquid,gasliquidadsorptionspectroscopymeasuring(differentcationadsorbsdifferentwavelengthoflight)24a)AADS(AtomAdsorptionSpectroscope)Mainlyusedtodeterminemicroelements(aboutallelementsintheElementTable)Fromgeneralconcentrationtomicro-concentration(%wttoug/g)25b)ICP(Plasma)Mainlyusedtodeterminemicrotohintelements(mostoftheelementsintheTablecanbedetermined)(ug/g---ng/g)262.1.3RadiatingSpectroscopelightsourcesolidsamplesecondlight(thewavelengthofthe2ndlightchangesaccordingtothekindoftheelementsinthesolidsample)---measuringthe2ndlightwavelength,sothekindsandthecontentsoftheelementsinthematerialcanbedetermined.27a)xrayFluorescenceSpectroscope(XRF)Generaltomicroconcentration(%wt—ug/g).Lightsource:xraywithcontinueswavelength.Sample:solid.theelementsfromNa11-U92.butcannotdistinguishthedifferentchargesofthesameelement:Fe2+andFe3+…28b)XrayPhotoelectronSpectroscope(XPS)Mainlytoidentifytheelements(qualitative).Itcandistinguishdifferentenvironmentsofthesameelement.OinCO3andinSiO4andinH