材料研究法方法课程 1 材料研究方法综述

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leixinrong2012@126.comcode:leixinrongEmail：xrlei@手机Q:619836585微信：xrleiCUG敬请不要随便删除信箱中的内容，谢谢！2Al2O3MgOSiO2OptionalratioheatingRawmaterial

singleelementmaterialAl:Aluminum(Cubic)Mg:Magnesium(Cubic)Mg:Magnesium(Hexagonal)Si:Silicon(Cubic)Si:Silicon(Hexagonal)Si:Silicon(Monoclinic)

3

Al-oxidesAl2O3

CorundumAl2O3RubyAl2O3CubictypeAl2O3HexagonaltypeAl2O3TetragonaltypeAl2O3

Orthohombictype…About30types

Mg-oxidesMgO

Periclase(Cubic)MgO(Cubic)MgO2(unknown)MgO4(Tetragonal)4types4

Mg-Al-oxidesMgAl2O4

SpinelMg-Al-OMgAl26O40Mg0.866Al1.830O3.611Mg0.388Al2.408O4Mg0.36Al2.44O4

Crawfordite(Mg0.4Al0.6)Al1.8O4……

Al-Si-oxidesAl2SiO5

sillimaniteAl2SiO5kyaniteAl2SiO5andalusiteAl2SiO5sillimanite……5

Al-Si-oxidesAl2SiO5

sillimaniteAl2SiO5kyaniteAl2SiO5andalusiteAl2SiO5sillimanite……6

Mg-Al-Si-oxidesMg2Al4Si5O18CordieriteMg3Al2Si3O12PyropeMg2(Al4Si5O18)CordieriteMg4Al10Si2O23sappirineMg2Al4Si5O18indialiteMg2Al3(Si3Al)O10O8chlorite…About50kindsTotally300-400typesofphase7Purpos：Todetermine(1)thechemicalcomposition,(2)thestructure,(3)thesurfacemorphology,(4)thephysicalandchemicalpropertiesofthematerials.8Outline1.1Chemicalcompositionanalysis:

todeterminethekindsandthecontentsoftheelementsinamaterial.

Qualitativeand

Quantitative9QualitativeandQuantitative（定性分析和定量分析）Qualitativeanalysisisusedtodeterminethekindsofcationsandanions（阳离子和阴离子）

inasamplesubstanceQuantitativeanalysisisusedtodeterminethekindsandthecontentsofcationsandanionsinasamplesubstance10Describingthechemicalcomposition:Weightconcentration:forsolid,liquid

Generalelement%wt

MicroElement:ug/g(g/t)(ppm)10-6

Super-micro:ng/g(ppb)10-9

HintElement:pg/g(ppt)10-12

Volumeconcentration:forliquid,gas

General:mol/L

Micro:mmol/L11ExpressingtheChemicalCompositiona)Formetal,singleelementmaterial,

sulfide（硫化物）,andsomeothermaterials

thattheirionsarenotoxygen.

ExpressingasElementcontent.

Iron(钢材):Fe:99.00%wt,C:1.00%wt

Pyrrhotite(磁黄铁矿)(Fe1-xS):

Fe:63.00%wtS:36.00%wtNi:0.50%wt12ExpressingtheChemicalCompositionb)Foroxide(氧化物),Silicate(硅酸盐),andsomeothermaterialsthattheirionisoxygen(carbonate碳酸盐,sulfate硫酸盐…).

Whenexpressingtheircompositions,generallyasoxidetypes13Forexample:Orthoclass钾长石(KAlSi3O8):

K2O15.13%wtSiO263.51%wtAl2O318.99%wt

Na2O1.34%wtCaO0.13%wtFe2O30.09%wt

Calcite方解石(CaCO3):

CaO55.03%wtFeO0.12%wt

MgO0.22%wtCO243.97%wt14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:35.01

3个有效位时等于:35.014

4舍6入,5单双(奇进偶不进)

如：小数后取两位：

35.045---35.04

35.035---35.04

35.0451---35.05151.2structuralAnalysis: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)16Forexample:C(Carbon):

canbegraphite(石墨)orbediamond（金刚石）,becausetheyhavedifferentstructure(atomarrangementisdifferent)

SiO2：

αQuartz（石英）,βquartz,……

Al2[SiO4]O:

Andalusite(红柱石)

Kyanite(蓝晶石)17Describingthestructure:Crystalsystem:

cubic（立方晶系）,tetragonal（四方晶系）,orthorhombic（斜方晶系）,monoclinic（单斜晶系）,triclinic（三斜晶系）,hexagonal（六方晶系）,triogonal（三方晶系）,

Symmetry（对称）:

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,½,½,½.181.3Morphological（形态）properties(Surfaceobservation)MorphologicalpropertiesincludeMacro（宏观）,Micro（微观）,Super（超微）Microproperties.

Macro-bynakedeyes（裸眼）.

Micro-bymicroscope,electronmicroscope…

SuperMicro-Scanningtunnelingmicroscopy（STM）

Atomicforcemicroscopy（AFM)19Toobservetheshapeoftheparticles,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)201.4Analysisofphysicalandchemicalproperties

Including

Thermal,Light,electricity,mechanics,etc.212.AnalyzingMethods222.1ChemicalComposition

2.1.1WetChemicalAnalysis:

湿法化学分析

solid,liquid,gasliquidchemicalreactioncalculatingchemicalanalyzingresult

23Silicate（硅酸盐）analysis(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

（一般小数点后保留两位有效数字）.242.1.2Absorptionspectroscope(吸收光谱）

(Instrument（仪器）analysis)

Generalconcentration(%wt)tomicro(ug/g)andalsotohintconcentration(ng/g)solid,liquid,gasliquidadsorptionspectroscopymeasuring(differentcationadsorbsdifferent

wavelengthoflight)25a)

AADS(AtomAdsorptionSpectroscope)

Mainlyusedtodeterminemicroelements(aboutallelementsintheElementTable)

Fromgeneralconcentrationtomicro-concentration(%wttoug/g)

26b)

ICP(Plasma)（等离子）

Mainlyusedtodeterminemicrotohintelements(mostoftheelementsintheTablecanbedetermined)

(ug/g---ng/g)272.1.3

radiationspectrum（辐射光谱）lightsourcesolidsamplesecondlight(thewavelengthofthe2ndlightchangesaccordingtothekindoftheelementsinthesolidsample)---measuringthe2ndlightwavelength,sothekindsandthecontentsoftheelementsinthematerialcanbedetermined.28a)

xrayFluorescenceSpectroscope(XRF)（荧光光谱）

Generaltomicroconcentration(%wt—ug/g).

Lightsource:xraywithcontinueswavelength.

Sample:solid.

theelementsfromNa11-U92.butcannotdistinguishthedifferentchargesofthesameelement:Fe2+andFe3+…29b)

XrayPhotoelectronSpectroscope(XPS)

（光电子能谱）

Mainlytoidentifytheelements(qualitative).

Itcandistinguishdifferentenvironmentsofthesameelement.OinCO3andinSiO4andinH2O.

Sourcelight:xraywithcertainwavelength.

Sample:solid.30c)

IsotopeAnalysis（同位素分析）:

Todeterminetheratioofthedifferentisotopesofthesameelement.Mainlyusetodeterminetheageofthesample.

Sourcelight:Proton（质子）

H<100y

14C<50,000

32Si<n00,000

36Cl<n,000,000

129I<*,000,000

K/Ar<m,000,000

Rb/Sr,Sm/Nd,

U/Pb<n00,000,000StableisotopeRadiatingIsotope312.1.4othermethods

a)

ElectronProbeMicroscopic（electron-probemicroscopy电子探针显微）analysis

SimilartoXRF.Butthelightsourceiselectronbeam,andtheanalysisonlybeinaverysmallregion.Soitiscalledmicro-regionchemicalanalyzingmethod).

Twokindsofresult:WavedisperseSpectroscopy

EnergyDisperseSpectroscopy

Elementrange:Na11-U92

Concentrationrange:%wt–ug/g

(Italsocannotdistinguishthedifferentchargesofthesameelement,forexample:Fe2+andFe3+).32b)

AES（Augerelectronspectroscopy）

俄歇电子谱仪

SimilartoEPMA,butonlydeterminethechemicalcompositionoftheverysurfacelayer.

c)

ElementAnalyzer:

Organicanalysis,C,H,O,N,S:Quantitative

33d)

Chromatogram（色谱）

Twokinds:gas,liquid:

C,H,O,N,SQualitative.

Mainlytodeterminethestructureoftheorganic.

Forexample,thelengthofthecarbonchain.

d)

MossbuareSpectroscope:

穆氏鲍尔谱

Todeterminetheratioofthedifferentchargesofthesame

element.Forexample,Fe2+/Fe3+…34通常我们所说的物质的组成，有两个方面的含义：一是化学组成，一是物相组成。

例如一种材料在描述物质组成时，说明如下：SiO2：63％wt，Al2O3：37％wt。该如何理解该种材料的物质组成？1：化学成分：Si、Al、O2：物相种类：（1）石英相、刚玉相（2）单质硅、单质铝＋上（3）铝硅酸盐＋上

……2.2StructureAnalysis

352.2.1Xraydiffraction(XRD)

(X射线衍射)

a)

singlecrystalmethod:

Mainlytodeterminethestructureofthenewmaterial

b)

Powdercrystalmethod:

Mainlytodeterminethemineral（矿物）phase,qualitativeorquantitative.Onlyvalidtothecrystal.362.2TransparentElectronMicroscope(TEM)（透射电镜）

Todeterminethestructureofthesampleinaverysmallregion.(nmregion)372.2.3Infrared（红外线）Spectroscope(IR)（红外）:

Todeterminetheexistenceofthechemicalbonds（化学键）inthesample(material),alsocanbeusedtodeterminethemineralphase(differentmineralhasdifferentchemicalbonds:theirkindsandstrength).

Adsorpti