钢中夹杂物的常规定性分析

第27卷第4期

2007年4月

冶金分析MetallurgicalAnalysis

V01.27.No.4April,2007

{II

文章编号:1000—7571(2007)04—0001—06

RoutinequalitatiVeanalysisof

inclusionsinsteel

研究与试验报告

蒂TORTOREToGiampietro‘,SCIABOLETTADomenico,

ROTICIANISilvio

(ThyssenKrupp

Acciai

SpecialiTemi,Temi,Italy)

Abstr舵t:MoSt

microscopy

on

investigationsofinclusionsandprecipitateswere,andstillare,donebyoptical

polishedsteelsurfaces.Improvementoftheresolutionofpulsediscriminationanal—

ysis-opticalemiSsionspectrometry(PDA—OES)isexpectedinthe∞mingyearS.Size,numberandspatialdistribution

can

berecorded.Duringautomaticrnonitoring,combinedwitheitherelectron

is

probemicro—analysis(EPMA)orPDA-OES,ap01ishedsteelsurface

shapeanditssurfacecharacteristicsteUthehistoryof

to

scanned.Althou曲area

not

and

perimeteroftheinclusionsisrecorded,derivationoftheirshapesis

evident.Theinclusion’s

particularinclusion.Thereforebeingableaboutinclusion

readthehistorymayresultinadditional

to

infomation

fo瑚ation,growth

and

evolution.Theaimofthisworkwasfind

correlationbetweenSEM/EDSanalysisandOES/

to

PDAtechniques.ThePDA—oEStechniqueswereusedstaillleSssteel,aSwell

aS

analyzequalitativelytheinclusionsin

or

incarbonsteel.Onthebaseofthisstudy,Semi—quantitative

quantita—

tiveanalysisoftheinclusionswillbeexpectedtorealizebyconsideringtheheightandtheintensity

ofthepeakswithpropercompa“SOnKeywords:

to

referencematerials.

opticalemissionspectroscopy;non—

stainlesssteel;pulSediscriminationanalysis;

meta¨icinclusions

CLCnumber:0657.63

D0cumentcode:A

ThesteelindustryisfacedwiththechaUengeofproducinghigherqualityandcleanersteel,while

increasing

也eirdeannessindex.

Mostim怪缸gatiOnsofineIusionsa11d

were,aJldstiUare,dDnebyoptical

productivity.

onthisbase

significant

micI唧y

can

precipitates

on

pol—

progresshasbeenmadeintheanalySisofironand

iShedsteels1】rfaoes.

FH瑚1960on啪rds

elec臼Dnmi—

steel:sampleanalysistime,sensitivity,

andaccuracy

precision

clDscopybecamewid爱pread.Thisnotodye陇出lesin一

haveallbeensubstantiaUyimpt.oved

inthelastyears.

嘣i野monlaIgerm碰;mfications,butiteasilybeO(m=1:bined、^,ith删yticaltec:h11iques,calledelec旬Dn

at

Adl旧noedsClftwareapplicatjoninopticalerlliSsliCln

spectrometry,、ⅣitlltheaoquiSitionoft11e1ightintensity

p出rni静砌灿(EP凇)[1-2].In

small

EPMAthe

6ktmn

b哪,which

iSinScarulingrIⅪDdeuSed

鲥tted

byeachsin西esparkoft11ediScharge,opensforimaging,西v签riSe

t0“sSiIm

call

ofX-myS谢th

pr爱蛇nt.

H】ost

newgoalsintheapplicationofthiStEdlmque.Optical

wavelen戥hScharacteristicfbrt11eeleInentSTheapplic撕onofof出e

p;lrmneters

an

蹦SSion

Sple(=t1_cIⅡ1eterscoddnotodydisplay,within

EM厄PMA

chamctedSe

fewSeamds,the

d戚cal

O(mlp商tion

of

metal蛐一

printout,

and

describingt11eSteddediness.USing

ples,butaLts0,inreal6meandonthe

valllableinfbtTnation

saIlle

back_scatteredelectronsfbrimagingtheinduSionSshaw

ab珈lt小ejrindl】sion

o()ntent

Si鲥ficallt

00ntrast

to乱pohsheds渊“缸.The

Reoeiveddate:2006一09—16

Bio呻phy:GianlpietroTortoreto(1947一)。male。Ph.D。Laboratories

万方数据

mail:gi锄tof@1ibem.it.

Manager,ThyssenKrupp

Acciai

Speciali

Terni。E—

一1一

第27卷第4期2007年4月

冶金分析

V0l・27・No・4

MetauurgicalAnalysiS

April,2007

large

c0咖aSt

betweens乜eel

m缸x

a11dinclusions

en—

ablesautomaticmom幻ringif

sanlpkm0、唧mentsys—

t锄is

attached.Number,diameterandpedm酏erd

indusionscc疽TIbined、耐thrnicrpanalyses咖bereoDrd—

ed.Despiteiheauto姐ticmom砸ngthemetllodiSrd—

ativdvSlowdue

to

the

ti雠nec联;s奶7

f6f

accLlrate删一

ysis.

Spark—S0urce

optical

“ssion

Spec心mleny

((娅S),wmch

iS

s协dardforbulkstedanal姆s,∞m—

binedwithpulse

dbcri耐nationanalysis(PDA)haS

re—

cendybeendevelopedandismuchfaSterthanE ̄P—

MA[3—4|.In()ESPlDA,the

plaSnlacreates

ernissiC憷

of

li{出t、^,ith

wavden础scharactedsticfortheeIanents

pn葛ent.The

plaslm

is

producedduringelectricdis—

char_ge.Sincet11e

area

affectedbythe

pl猢is1arger

than吐眦of

an

dectmn

b咖for

EPⅣ睑,雠resolu—

tionofOESPDA

iS舢ch

less妇forEPMA,e.g.

30一50脚and

1—5

pm,re{;pectivd,5q].Inlp聊e—

m∞tdd旋Te9011】tion

d(黔PDAis镪【pe魄edh

the

∞mingyears.Size,mmiberandSpa6aldis试butioncan

be

re咖dod【9—10j.

AnalySis

are

performed

on

singleinstrument

at

clearlylower

costs,

in

comparison

to

existing

techniauesforsteelcleannesswhichare

time

con—

sumingand

expensive(SEM/EDSMicrograph).

AnOESmethodtoanalyseindusionsinstain—

lesssteelispresentedinthis

paper,acr.oss

study

ofthelightemittedbyeachsinglespark.Graphsofthe

overlappingof

the

lightsofelements,

con—

stituentoftheinclusions,areshowed.

Theaimof

our、∞rk

waStoanalySeexpected

differentphasesofoxides,carbidesandnitritesin

steelin

faStway,togivemore

infomation

tothe

productionandqualitycontr01.Atthe

momentitis

not

possible

quantitativeanalySis,wedonothave

referencematerialswitha

certifiedvalueofinctu—

sions,

nevertheleSs

qualitative

detemination

of

them

can

bealsouseful.

Theanalyticalprogramscan

beconfigured

aS

well

as

claSSicalpro罾rams,eachelement

canbecal—ibratedanddriftcorrected,theirresults

can

bedis-

played,stored,printedanddistributed,datahan—dlingakorithms

can

beeasilyselected

or

plugged

intothesoftware.

万方数据

一2—1

Experimental

IncIusiondetectionandanalysisweredone

un—

der

scanning

electron

microscope

SEM/EDS

CambridgeMod.with

tungsten

wiretodetectand

analyseallsecondphaseparticlesthatwereVisible

at

magnificationof1,000×.S涵ark—inducedopticalemission

spectroscopy

is

∞mmonlv

usedtodeterminethenominalchemistry

ofconductivesolidspecimens.

Inthiswork,

an

opticalEmissionSpectrometerARL4460ofThe卜

rno(乃rp.wasused.

Cbrrespondingopticalemissionintensityspec—

tra

can

berepresented

as

densityfunctionsobtained

byaccumulatingthenumberofpulSeSineachclass

ofintenSityallowedbythephotomultiplierSand

aS・

sociatedelectronicchain.

Thesespectra

are

usually

very

noisybecauseofsvstem

resolutionandanalysed

pulse

number

(1,500)limitations.

As

consequence,they

ex。

hibitimportantfillingdefects

atSomeintenSityleV。

els,alongwith

exceSS

fillings

at

otherleVels.

Inclusionsprecipitation

The{irst

st印doⅢre辩archwas幻ve《y,by

op—

ticalandscandng

inclusions

instajnIess

Steel

SaI]啊es.‰of伽dd删

dect姒1ical

midⅨ∞py,theoOilS,afbera

sellsitizing

them】al

tri舭nt

e)c成utedm

la_bOfat。fy

t0

predpi协tethephases,areshowed.

ADhotoofchromiumcarbides,obtainedafter

SenSitisingat675℃for1handat

magnification

of200X,isreportedinF谵.1:

Fig.1

se瞄iti髓dmicr憾tr眦ture(at675℃for

h)

Of

typic蚰austeniticstainlesss“埒l

(withtheevidence0fchmmiumc盯bid髂

M23c6

p陀cipitat酋)

Thefollowingfigure(Fig.2)referS

toto

ansee

EDS,

are

printed.From

theresults

we

can

say

austeniticstainlesssteelwhereitispossibleinclusions

whose

analysis,

thatthemaincompositionoftheinclusions

isbased

on

present

performedby

SEM/oxidesofA1,(、aandSi.

Fig.2

oxid鹤inclusionsina吣teniticstainIesssteeIarIdEI'sanaIysis

Fig.3

Thesameconclusions

can

oxid鹤incIusionsinausteniticstainIe蟠st∞landEDS蛆alysisbedroppeddownfromthefollowingsample.

InF培.4,anausteniticstainlesssteelstabilizedwithTiisreported,inthissamplewefoundinclu—sionsofTiNaccordingto

SEM/EDSanalySis。

Inconclusionthedistributionoftheindusionsindifferent

sampleswereanalysedby

SEM厄DS

can

micrOgraph.

Fromtheanalysisobtained,we

understandthatthe

are

followingoxidesandnitrideS

the

maincomponentsoftheinclusions:Cao,

Si02,A1203,TiN.

Wedid

not

considerthe

are

presence

ofFeandCr

oxidesbecausethey

l耗.4

themainconstituentsofthe

on

nt蛐i哪疵ridei眦I璐io璐in卸姚litic咖IIle略

titaniumandEDSanalysis

steelanalvsedandcouldinterfereanalysis.

SEM/EDS

steeIstabilizedby

万方数据

一3

第27卷第4期2007年4月

冶金分析v文27,No.4

April,2007

MetallurgicalAnalysis

IncIusionsanalysisbyoES

onceidentifiedthephases,by

highintensitypulsescouldcorrespondtoelements

containedininclusionswhenthev

and

anyto

arenot

due

to

SEM/EDS

kindofLABpollution.

Thechosenparameter

optical

Microscopy,we

startedthedetermination

indicatehighintensitypulsesistheaveragevalue

ofthembyOpticalEmissionSpectrometry.

Fmmthefollowinggraphs,whereeachsingle

sparkis

reported,wein

the

can

addedbythreetimesofstandarddeviationofthe

ones

||一^ihindicationofansparks.||Anof1argersizeof

oⅣer

assumethattheinclu.

theinclusionsisgiven

derofsixFig.5

or

thisreference

value(or—

In

an

sionsread

sampl毛sby

SEM厄DS

are

alSoninetimesofstandarddeviation).

readbyOES.

Thelowintensitypulsescorrespondtothe

sponse

re.

graph

indicating业03

inclusionsin

austeniticstainlesssteelisreported.Theoverlaps

ofelementsinsolutioninthemetalandthe

60∞

55∞50∞4S∞●—∞0

of02and趾pulseSindicatethepresence

of砧203.

3册

3∞D

2枷

2∞O

1脚

5∞

5∞

.{f.IJ|lJL』血I队,。u}J~一,“。…...。。LL血lu止.L止.-l~

…-”。’r

1’

湖枷

’’…rT…。n“…■…1-’r1Tr’r_P。r’-…'■’叮l‘■’…”’1●’'。’1—111I

嘲8∞’肋1抽’椭1枷1枷2彻

灿山

”r_…。‘1j’胛T"

“I山II111山』柚idlI山。-.ILk|I|-川.1.山

l’I”,’『r’1’I"’_

■nH7Ir

r。1-。-1啊'T-r’1I『-

'_’’’’叩1”1■

Fig.6

晰8∞

of

Typical粕alysis

steel

tit粕ium

nitrideincI晒io璐in

f电州ticstainI嘟

stabili跹dbytit粕iumbyoES(TiupNdown)

万方数据

专;万馨铲T昧T。R啪Qam。tetro,etd.勋utineauatt圳vea砌粥ts甜inc-us岫s

In

tnstee-

V01.27.No.4ADril,2007

sampleof

ferriticstainless

to

see

steel,

aS

InF遮.7,、Ve

call

see,twodjfferemoverhpping

showedinFig.6,itisalsopossible

ence

thepres—ofthepea:I【sofsdiO。nandoxygenat也elowersideof

ofTiN.

sparkmmiberst11at朗叩hasizeSthe

presenoe

of

siQ.

12脚

11咖10咖9J啪

8埘

7∞06.O∞5.0∞

3脚2脚’脚

●.∞O

r池L从1.IJl|…lI-ILI

.。lJj¨ll也“…I虬.L。h。l。。.:。|【J

'脚

1瑚

1枷

1枷

1枷

2咖

再电.7

PDA蛐alysis

spark

0f

Ca锄旧们碘}啪si弘蚰pIotted

upo

vs.

number(Ca

ox—

down)

We

didn’texactlyknowifaggregatesof

present

overlappingofthe

suggest

peaksofAlandSithatcould

an

idescouldbe

reaS0n

inthe

theinclusions.Fbrthis

of

our

thepresenceof

aggregate

or

clusterof

weexamined

reSponse

samples

an

sihcates(withstoichoiometryA12()3一Si()2).

andinsomeofthem,itwaspossibletofound

日6‘2De

6●2

枷蜘e∞嘲

Fig.8c盯bon

TypicaI粕alysis

in

of

chr帅ium

c盯bide

obtained

bythesignaIof

oES蛐aIysis(evidenceofIargerinte璐itypeab)andpu№in-

te砸itydistribution(hisbogram)ofc盯bonsignalsofehromiumcarbidesindusiO璐

FinanyinF谵.8,fI.omthesignalofcarbonof

an

PDA帆st∞1

with

quency

ofpeaksofCdeviation

over

the

average

plusthree

of

austeniticstainlesssteel18/8sensitised,thefre—standardcould

justify

the

presence

万方数据

5——

第27卷第4期冶金分析V。1.27.No.42007年4月

MetaUurgicalAnalySis

APril,2007

chromiumcarbide(Cr23C6).

Aboutthehigher

995.

sparknumberpeaks,theycouldrepresent

poSsi—

[3]PissenbergerA,Pissenberger

E.AutomaticCleanness

bleevidenceof

an

aggregatesofcarbide.

Instain—

Detemination

of

Pmduction

Sampleswith0ES/’PDA,

lesssteelscarbonitrides

as

well

7th

as

carbidescouldbe

J.Angeli(ed.):ProceedingsInternat[c].work—

and

present,we

are

stillinvestigatingon

theiridentifi—

shopPmgresSinAnal”icalChemistryintheSteelMetalIndustries,2006.

cationbothby

SEM/EDS

andbyOES.

[4]H哪merlin

M,MeillandaR,Falkb

H,et

a1.Applica—

4ConclusiOns

tionof

vacuumultmvioletlaSer—inducedbreaklown

spec—

trometryforsteelanalysiscompariSon谢thspark—optical

onthebaseoftheresultsobtaineditispossi—

锄iSSiollspectr㈨etry[J].SpectrochimicaActa:Part

B,

ble

tosay

thattheoES

can

beusedtoanalyse,in

2001,56(6):661—669.firststep,theinclusionspresentinstainlesssteel,

[5]RocaboisP,LehmannJ,Gaye

H,et

a1.Kineticsofpre—

as

wen

as

incarbonsteel[1].

cipitation

ofnon—metallicinclusionsduringSolidificationof

Of

courSe

themethod,abSOlutelyfast,isonly

steeI[J]。JoumaIofCryStaI

Growth,1999,198/199:

838—843.

qualitative.Cbnsideringtheheightandtheintedsi—

[6]FalkH,Wintjens

P.Evaluationof

Single.Sparksand

its

ty

ofthepeaks,after

proper

compariSonwithref—

Applicationsto

the

EvaluationofInclusions[J].Joumal

erence

materialsadhocprepared,thesecondstep

0fCrystal

Gro叭h,1999,413—419.

ofthisstudy,couldbe

semi—quantitative

or

quan—

[7]MeillandR,et

a1.Rapid

CharacterisationofHetero—

titativeanalysisoftheinclusions.

geneities(Inclusionsand

Segregation)bySpectralTech—

References

niques[J].JournalofCrystalGfowth,1999,420一427.

[8]Jo谢tt

R.Rapid

Detemination

ofsteelCleanliness[C].

[1]MullerE,ZuberC,B?hlenJM.on—Linespark—DAT

ECSC

Project72lO—GD/806FinalReport,1994.

fbrultimateeIementalanalvsisandadditionalmetalschar—

[9]MathyH,TusSetV,LamberigtsM.AnEvaluationof

acterization

with

0pticalEmissionSpectroscopy[Z].

SulphideIndusionContentAssessmentMethodsIn、,ac—ThermoARLAppliedResearchLaboratories,2006.

uum—ProcessedSteels,2006.

[2]MullerG,StahnkeF,Bleiner

D,Faststeel—cleanness[10]10。sta

A,silva.Th咖10dynamjc

aspectS

ofinduSilm∞画一

characterization

bymeansofIaser—assistedplasmaspec—ne刮119insteels[J].RareMetais,2006,25(5):412—

trametricmeth()ds[J].Talanta,2006,70(5):991—

419.

钢中夹杂物的常规定性分析

TORTORETOGiampietro,SCIABoLETTADomenico,RoTICIANISilvio

(ThyssenKrupp

Acciai

SpecialiTerni,Temi,Italy)

摘要:对于钢中夹杂物的研究,目前大多数工作是采用光学显微镜测量抛光的钢样表面的方

法实现的。今后若干年里,脉冲分布解析原子发射光谱法(PDA-oES)的分辩率有望得到提高,可以获得夹杂物的尺寸、颗粒数以及空间分布的信息。在应用电子探针微区分析(EPMA)或PD瓜OES技术的自动监控过程中,是对抛光的钢表面进行扫描分析。虽然可以获得夹杂

物的截面面积及其边界信息,但是这些夹杂物形状的成因却不明显。由于夹杂物的形状和表面特性可以揭示出某类夹杂物的形成过程,因此获知夹杂物的形成过程就可以得到夹杂物的

形成、生长和演变等相关信息。本文的目的就是研究钢中夹杂物分析中SEM侄DS技术和0ES/PI)A技术的相关性。应用PD艮OES技术对不锈钢及碳钢中夹杂物进行了定性分析。在此基础上,通过峰高和峰强度与参考物质的比较,将有望实现对夹杂物的半定量或定量分析。关键词:不锈钢;脉冲分布解析;原子发射光谱;非金属夹杂物

万方数据

第27卷第4期

2007年4月

冶金分析MetallurgicalAnalysis

V01.27.No.4April,2007

{II

文章编号:1000—7571(2007)04—0001—06

RoutinequalitatiVeanalysisof

inclusionsinsteel

研究与试验报告

蒂TORTOREToGiampietro‘,SCIABOLETTADomenico,

ROTICIANISilvio

(ThyssenKrupp

Acciai

SpecialiTemi,Temi,Italy)

Abstr舵t:MoSt

microscopy

on

investigationsofinclusionsandprecipitateswere,andstillare,donebyoptical

polishedsteelsurfaces.Improvementoftheresolutionofpulsediscriminationanal—

ysis-opticalemiSsionspectrometry(PDA—OES)isexpectedinthe∞mingyearS.Size,numberandspatialdistribution

can

berecorded.Duringautomaticrnonitoring,combinedwitheitherelectron

is

probemicro—analysis(EPMA)orPDA-OES,ap01ishedsteelsurface

shapeanditssurfacecharacteristicsteUthehistoryof

to

scanned.Althou曲area

not

and

perimeteroftheinclusionsisrecorded,derivationoftheirshapesis

evident.Theinclusion’s

particularinclusion.Thereforebeingableaboutinclusion

readthehistorymayresultinadditional

to

infomation

fo瑚ation,growth

and

evolution.Theaimofthisworkwasfind

correlationbetweenSEM/EDSanalysisandOES/

to

PDAtechniques.ThePDA—oEStechniqueswereusedstaillleSssteel,aSwell

aS

analyzequalitativelytheinclusionsin

or

incarbonsteel.Onthebaseofthisstudy,Semi—quantitative

quantita—

tiveanalysisoftheinclusionswillbeexpectedtorealizebyconsideringtheheightandtheintensity

ofthepeakswithpropercompa“SOnKeywords:

to

referencematerials.

opticalemissionspectroscopy;non—

stainlesssteel;pulSediscriminationanalysis;

meta¨icinclusions

CLCnumber:0657.63

D0cumentcode:A

ThesteelindustryisfacedwiththechaUengeofproducinghigherqualityandcleanersteel,while

increasing

也eirdeannessindex.

Mostim怪缸gatiOnsofineIusionsa11d

were,aJldstiUare,dDnebyoptical

productivity.

onthisbase

significant

micI唧y

can

precipitates

on

pol—

progresshasbeenmadeintheanalySisofironand

iShedsteels1】rfaoes.

FH瑚1960on啪rds

elec臼Dnmi—

steel:sampleanalysistime,sensitivity,

andaccuracy

precision

clDscopybecamewid爱pread.Thisnotodye陇出lesin一

haveallbeensubstantiaUyimpt.oved

inthelastyears.

嘣i野monlaIgerm碰;mfications,butiteasilybeO(m=1:bined、^,ith删yticaltec:h11iques,calledelec旬Dn

at

Adl旧noedsClftwareapplicatjoninopticalerlliSsliCln

spectrometry,、ⅣitlltheaoquiSitionoft11e1ightintensity

p出rni静砌灿(EP凇)[1-2].In

small

EPMAthe

6ktmn

b哪,which

iSinScarulingrIⅪDdeuSed

鲥tted

byeachsin西esparkoft11ediScharge,opensforimaging,西v签riSe

t0“sSiIm

call

ofX-myS谢th

pr爱蛇nt.

H】ost

newgoalsintheapplicationofthiStEdlmque.Optical

wavelen戥hScharacteristicfbrt11eeleInentSTheapplic撕onofof出e

p;lrmneters

an

蹦SSion

Sple(=t1_cIⅡ1eterscoddnotodydisplay,within

EM厄PMA

chamctedSe

fewSeamds,the

d戚cal

O(mlp商tion

of

metal蛐一

printout,

and

describingt11eSteddediness.USing

ples,butaLts0,inreal6meandonthe

valllableinfbtTnation

saIlle

back_scatteredelectronsfbrimagingtheinduSionSshaw

ab珈lt小ejrindl】sion

o()ntent

Si鲥ficallt

00ntrast

to乱pohsheds渊“缸.The

Reoeiveddate:2006一09—16

Bio呻phy:GianlpietroTortoreto(1947一)。male。Ph.D。Laboratories

万方数据

mail:gi锄tof@1ibem.it.

Manager,ThyssenKrupp

Acciai

Speciali

Terni。E—

一1一

第27卷第4期2007年4月

冶金分析

V0l・27・No・4

MetauurgicalAnalysiS

April,2007

large

c0咖aSt

betweens乜eel

m缸x

a11dinclusions

en—

ablesautomaticmom幻ringif

sanlpkm0、唧mentsys—

t锄is

attached.Number,diameterandpedm酏erd

indusionscc疽TIbined、耐thrnicrpanalyses咖bereoDrd—

ed.Despiteiheauto姐ticmom砸ngthemetllodiSrd—

ativdvSlowdue

to

the

ti雠nec联;s奶7

f6f

accLlrate删一

ysis.

Spark—S0urce

optical

“ssion

Spec心mleny

((娅S),wmch

iS

s协dardforbulkstedanal姆s,∞m—

binedwithpulse

dbcri耐nationanalysis(PDA)haS

re—

cendybeendevelopedandismuchfaSterthanE ̄P—

MA[3—4|.In()ESPlDA,the

plaSnlacreates

ernissiC憷

of

li{出t、^,ith

wavden础scharactedsticfortheeIanents

pn葛ent.The

plaslm

is

producedduringelectricdis—

char_ge.Sincet11e

area

affectedbythe

pl猢is1arger

than吐眦of

an

dectmn

b咖for

EPⅣ睑,雠resolu—

tionofOESPDA

iS舢ch

less妇forEPMA,e.g.

30一50脚and

1—5

pm,re{;pectivd,5q].Inlp聊e—

m∞tdd旋Te9011】tion

d(黔PDAis镪【pe魄edh

the

∞mingyears.Size,mmiberandSpa6aldis试butioncan

be

re咖dod【9—10j.

AnalySis

are

performed

on

singleinstrument

at

clearlylower

costs,

in

comparison

to

existing

techniauesforsteelcleannesswhichare

time

con—

sumingand

expensive(SEM/EDSMicrograph).

AnOESmethodtoanalyseindusionsinstain—

lesssteelispresentedinthis

paper,acr.oss

study

ofthelightemittedbyeachsinglespark.Graphsofthe

overlappingof

the

lightsofelements,

con—

stituentoftheinclusions,areshowed.

Theaimof

our、∞rk

waStoanalySeexpected

differentphasesofoxides,carbidesandnitritesin

steelin

faStway,togivemore

infomation

tothe

productionandqualitycontr01.Atthe

momentitis

not

possible

quantitativeanalySis,wedonothave

referencematerialswitha

certifiedvalueofinctu—

sions,

nevertheleSs

qualitative

detemination

of

them

can

bealsouseful.

Theanalyticalprogramscan

beconfigured

aS

well

as

claSSicalpro罾rams,eachelement

canbecal—ibratedanddriftcorrected,theirresults

can

bedis-

played,stored,printedanddistributed,datahan—dlingakorithms

can

beeasilyselected

or

plugged

intothesoftware.

万方数据

一2—1

Experimental

IncIusiondetectionandanalysisweredone

un—

der

scanning

electron

microscope

SEM/EDS

CambridgeMod.with

tungsten

wiretodetectand

analyseallsecondphaseparticlesthatwereVisible

at

magnificationof1,000×.S涵ark—inducedopticalemission

spectroscopy

is

∞mmonlv

usedtodeterminethenominalchemistry

ofconductivesolidspecimens.

Inthiswork,

an

opticalEmissionSpectrometerARL4460ofThe卜

rno(乃rp.wasused.

Cbrrespondingopticalemissionintensityspec—

tra

can

berepresented

as

densityfunctionsobtained

byaccumulatingthenumberofpulSeSineachclass

ofintenSityallowedbythephotomultiplierSand

aS・

sociatedelectronicchain.

Thesespectra

are

usually

very

noisybecauseofsvstem

resolutionandanalysed

pulse

number

(1,500)limitations.

As

consequence,they

ex。

hibitimportantfillingdefects

atSomeintenSityleV。

els,alongwith

exceSS

fillings

at

otherleVels.

Inclusionsprecipitation

The{irst

st印doⅢre辩archwas幻ve《y,by

op—

ticalandscandng

inclusions

instajnIess

Steel

SaI]啊es.‰of伽dd删

dect姒1ical

midⅨ∞py,theoOilS,afbera

sellsitizing

them】al

tri舭nt

e)c成utedm

la_bOfat。fy

t0

predpi协tethephases,areshowed.

ADhotoofchromiumcarbides,obtainedafter

SenSitisingat675℃for1handat

magnification

of200X,isreportedinF谵.1:

Fig.1

se瞄iti髓dmicr憾tr眦ture(at675℃for

h)

Of

typic蚰austeniticstainlesss“埒l

(withtheevidence0fchmmiumc盯bid髂

M23c6

p陀cipitat酋)

Thefollowingfigure(Fig.2)referS

toto

ansee

EDS,

are

printed.From

theresults

we

can

say

austeniticstainlesssteelwhereitispossibleinclusions

whose

analysis,

thatthemaincompositionoftheinclusions

isbased

on

present

performedby

SEM/oxidesofA1,(、aandSi.

Fig.2

oxid鹤inclusionsina吣teniticstainIesssteeIarIdEI'sanaIysis

Fig.3

Thesameconclusions

can

oxid鹤incIusionsinausteniticstainIe蟠st∞landEDS蛆alysisbedroppeddownfromthefollowingsample.

InF培.4,anausteniticstainlesssteelstabilizedwithTiisreported,inthissamplewefoundinclu—sionsofTiNaccordingto

SEM/EDSanalySis。

Inconclusionthedistributionoftheindusionsindifferent

sampleswereanalysedby

SEM厄DS

can

micrOgraph.

Fromtheanalysisobtained,we

understandthatthe

are

followingoxidesandnitrideS

the

maincomponentsoftheinclusions:Cao,

Si02,A1203,TiN.

Wedid

not

considerthe

are

presence

ofFeandCr

oxidesbecausethey

l耗.4

themainconstituentsofthe

on

nt蛐i哪疵ridei眦I璐io璐in卸姚litic咖IIle略

titaniumandEDSanalysis

steelanalvsedandcouldinterfereanalysis.

SEM/EDS

steeIstabilizedby

万方数据

一3

第27卷第4期2007年4月

冶金分析v文27,No.4

April,2007

MetallurgicalAnalysis

IncIusionsanalysisbyoES

onceidentifiedthephases,by

highintensitypulsescouldcorrespondtoelements

containedininclusionswhenthev

and

anyto

arenot

due

to

SEM/EDS

kindofLABpollution.

Thechosenparameter

optical

Microscopy,we

startedthedetermination

indicatehighintensitypulsesistheaveragevalue

ofthembyOpticalEmissionSpectrometry.

Fmmthefollowinggraphs,whereeachsingle

sparkis

reported,wein

the

can

addedbythreetimesofstandarddeviationofthe

ones

||一^ihindicationofansparks.||Anof1argersizeof

oⅣer

assumethattheinclu.

theinclusionsisgiven

derofsixFig.5

or

thisreference

value(or—

In

an

sionsread

sampl毛sby

SEM厄DS

are

alSoninetimesofstandarddeviation).

readbyOES.

Thelowintensitypulsescorrespondtothe

sponse

re.

graph

indicating业03

inclusionsin

austeniticstainlesssteelisreported.Theoverlaps

ofelementsinsolutioninthemetalandthe

60∞

55∞50∞4S∞●—∞0

of02and趾pulseSindicatethepresence

of砧203.

3册

3∞D

2枷

2∞O

1脚

5∞

5∞

.{f.IJ|lJL』血I队,。u}J~一,“。…...。。LL血lu止.L止.-l~

…-”。’r

1’

湖枷

’’…rT…。n“…■…1-’r1Tr’r_P。r’-…'■’叮l‘■’…”’1●’'。’1—111I

嘲8∞’肋1抽’椭1枷1枷2彻

灿山

”r_…。‘1j’胛T"

“I山II111山』柚idlI山。-.ILk|I|-川.1.山

l’I”,’『r’1’I"’_

■nH7Ir

r。1-。-1啊'T-r’1I『-

'_’’’’叩1”1■

Fig.6

晰8∞

of

Typical粕alysis

steel

tit粕ium

nitrideincI晒io璐in

f电州ticstainI嘟

stabili跹dbytit粕iumbyoES(TiupNdown)

万方数据

专;万馨铲T昧T。R啪Qam。tetro,etd.勋utineauatt圳vea砌粥ts甜inc-us岫s

In

tnstee-

V01.27.No.4ADril,2007

sampleof

ferriticstainless

to

see

steel,

aS

InF遮.7,、Ve

call

see,twodjfferemoverhpping

showedinFig.6,itisalsopossible

ence

thepres—ofthepea:I【sofsdiO。nandoxygenat也elowersideof

ofTiN.

sparkmmiberst11at朗叩hasizeSthe

presenoe

of

siQ.

12脚

11咖10咖9J啪

8埘

7∞06.O∞5.0∞

3脚2脚’脚

●.∞O

r池L从1.IJl|…lI-ILI

.。lJj¨ll也“…I虬.L。h。l。。.:。|【J

'脚

1瑚

1枷

1枷

1枷

2咖

再电.7

PDA蛐alysis

spark

0f

Ca锄旧们碘}啪si弘蚰pIotted

upo

vs.

number(Ca

ox—

down)

We

didn’texactlyknowifaggregatesof

present

overlappingofthe

suggest

peaksofAlandSithatcould

an

idescouldbe

reaS0n

inthe

theinclusions.Fbrthis

of

our

thepresenceof

aggregate

or

clusterof

weexamined

reSponse

samples

an

sihcates(withstoichoiometryA12()3一Si()2).

andinsomeofthem,itwaspossibletofound

日6‘2De

6●2

枷蜘e∞嘲

Fig.8c盯bon

TypicaI粕alysis

in

of

chr帅ium

c盯bide

obtained

bythesignaIof

oES蛐aIysis(evidenceofIargerinte璐itypeab)andpu№in-

te砸itydistribution(hisbogram)ofc盯bonsignalsofehromiumcarbidesindusiO璐

FinanyinF谵.8,fI.omthesignalofcarbonof

an

PDA帆st∞1

with

quency

ofpeaksofCdeviation

over

the

average

plusthree

of

austeniticstainlesssteel18/8sensitised,thefre—standardcould

justify

the

presence

万方数据

5——

第27卷第4期冶金分析V。1.27.No.42007年4月

MetaUurgicalAnalySis

APril,2007

chromiumcarbide(Cr23C6).

Aboutthehigher

995.

sparknumberpeaks,theycouldrepresent

poSsi—

[3]PissenbergerA,Pissenberger

E.AutomaticCleanness

bleevidenceof

an

aggregatesofcarbide.

Instain—

Detemination

of

Pmduction

Sampleswith0ES/’PDA,

lesssteelscarbonitrides

as

well

7th

as

carbidescouldbe

J.Angeli(ed.):ProceedingsInternat[c].work—

and

present,we

are

stillinvestigatingon

theiridentifi—

shopPmgresSinAnal”icalChemistryintheSteelMetalIndustries,2006.

cationbothby

SEM/EDS

andbyOES.

[4]H哪merlin

M,MeillandaR,Falkb

H,et

a1.Applica—

4ConclusiOns

tionof

vacuumultmvioletlaSer—inducedbreaklown

spec—

trometryforsteelanalysiscompariSon谢thspark—optical

onthebaseoftheresultsobtaineditispossi—

锄iSSiollspectr㈨etry[J].SpectrochimicaActa:Part

B,

ble

tosay

thattheoES

can

beusedtoanalyse,in

2001,56(6):661—669.firststep,theinclusionspresentinstainlesssteel,

[5]RocaboisP,LehmannJ,Gaye

H,et

a1.Kineticsofpre—

as

wen

as

incarbonsteel[1].

cipitation

ofnon—metallicinclusionsduringSolidificationof

Of

courSe

themethod,abSOlutelyfast,isonly

steeI[J]。JoumaIofCryStaI

Growth,1999,198/199:

838—843.

qualitative.Cbnsideringtheheightandtheintedsi—

[6]FalkH,Wintjens

P.Evaluationof

Single.Sparksand

its

ty

ofthepeaks,after

proper

compariSonwithref—

Applicationsto

the

EvaluationofInclusions[J].Joumal

erence

materialsadhocprepared,thesecondstep

0fCrystal

Gro叭h,1999,413—419.

ofthisstudy,couldbe

semi—quantitative

or

quan—

[7]MeillandR,et

a1.Rapid

CharacterisationofHetero—

titativeanalysisoftheinclusions.

geneities(Inclusionsand

Segregation)bySpectralTech—

References

niques[J].JournalofCrystalGfowth,1999,420一427.

[8]Jo谢tt

R.Rapid

Detemination

ofsteelCleanliness[C].

[1]MullerE,ZuberC,B?hlenJM.on—Linespark—DAT

ECSC

Project72lO—GD/806FinalReport,1994.

fbrultimateeIementalanalvsisandadditionalmetalschar—

[9]MathyH,TusSetV,LamberigtsM.AnEvaluationof

acterization

with

0pticalEmissionSpectroscopy[Z].

SulphideIndusionContentAssessmentMethodsIn、,ac—ThermoARLAppliedResearchLaboratories,2006.

uum—ProcessedSteels,2006.

[2]MullerG,StahnkeF,Bleiner

D,Faststeel—cleanness[10]10。sta

A,silva.Th咖10dynamjc

aspectS

ofinduSilm∞画一

characterization

bymeansofIaser—assistedplasmaspec—ne刮119insteels[J].RareMetais,2006,25(5):412—

trametricmeth()ds[J].Talanta,2006,70(5):991—

419.

钢中夹杂物的常规定性分析

TORTORETOGiampietro,SCIABoLETTADomenico,RoTICIANISilvio

(ThyssenKrupp

Acciai

SpecialiTerni,Temi,Italy)

摘要:对于钢中夹杂物的研究,目前大多数工作是采用光学显微镜测量抛光的钢样表面的方

法实现的。今后若干年里,脉冲分布解析原子发射光谱法(PDA-oES)的分辩率有望得到提高,可以获得夹杂物的尺寸、颗粒数以及空间分布的信息。在应用电子探针微区分析(EPMA)或PD瓜OES技术的自动监控过程中,是对抛光的钢表面进行扫描分析。虽然可以获得夹杂

物的截面面积及其边界信息,但是这些夹杂物形状的成因却不明显。由于夹杂物的形状和表面特性可以揭示出某类夹杂物的形成过程,因此获知夹杂物的形成过程就可以得到夹杂物的

形成、生长和演变等相关信息。本文的目的就是研究钢中夹杂物分析中SEM侄DS技术和0ES/PI)A技术的相关性。应用PD艮OES技术对不锈钢及碳钢中夹杂物进行了定性分析。在此基础上,通过峰高和峰强度与参考物质的比较,将有望实现对夹杂物的半定量或定量分析。关键词:不锈钢;脉冲分布解析;原子发射光谱;非金属夹杂物

万方数据


相关文章

  • 钢中夹杂物知识 1
  • 摘要:根据钢中非金属夹杂物的来源和分类,综述了鉴定钢中非金属夹杂物的方法和定量评级标准,并且给出了典型夹杂物的扫描电镜照片,分析了不同类型夹杂物的形成机理及其在光学显微镜下的基本特征. 随着现代工程技术的发展,对钢的综合性能要求也日趋严格, ...查看


  • 钢中夹杂物知识
  • 摘要:根据钢中非金属夹杂物的来源和分类,综述了鉴定钢中非金属夹杂物的方法和定量评级标准,并且给出了典型夹杂物的扫描电镜照片,分析了不同类型夹杂物的形成机理及其在光学显微镜下的基本特征. 随着现代工程技术的发展,对钢的综合性能要求也日趋严格, ...查看


  • 钢中非金属夹杂物的鉴定
  • 钢中非金属夹杂物的鉴定 发布者:北京普瑞赛司仪器有限公司 发布时间:2007-11-11 阅读:484次 尹安远,吴素君 摘要:根据钢中非金属夹杂物的来源和分类,综述了鉴定钢中非金属夹杂物的方法和定量评级标准,并且给出了典型夹杂物的扫描电镜 ...查看


  • 8非金属夹杂物
  • <钢材质量检验>单元教学设计 一.教案头 课题:教材:授课班级 非金属夹杂物检验 冶金工业出版社出版的<钢材质量检验>,页码109-111页.15冶金技术 能力(技能)目标 教学目标 课时:2学时知识目标 授课类型: ...查看


  • 304不锈钢表面锈蚀原因
  • 304不锈钢表面锈蚀原因 304奥氏体不锈钢(新标准的06Cr19Ni10钢.旧标准的0Cr18Ni9钢)由于其常温和低温下有良好的韧性.塑性.焊接性.耐腐蚀性及无磁性,广泛用于石油化工.冶金机械.航天航空.食品加工.仪器仪表.家用电器和五 ...查看


  • 轧机轴承的使用寿命
  • 轧机轴承的使用寿命 目录 一.影响轧机轴承使用寿命的因素 (一).基本额定寿命 (二).径向基本额定动负荷 (三).修正额定寿命 (四).油膜润滑参数 (五).密合度(待整理) (六).影响轧机轴承使用寿命的因素 二.轧机轴承的失效分析 ( ...查看


  • ATP002 金相高倍检验技术
  • 全国分析检测人员能力培训委员会 ATP002金相高倍检验技术 考核与培训大纲 第1版 文件编号:ATP002/A:2010-1 发布日期:2010年 8月 1 总则 1.1 目标 了解金相高倍分析和检验技术相关的基本概念和基础理论知识: 掌 ...查看


  • 复合材料的细观力学研究进展
  • 第28卷第3期 江西 科 学 V01.28No.3 2010年6月 JIANGXI SCIENCE Jun.2010 文章编号:1001-3679(2010)03-0354-05 复合材料的细观力学研究进展 刘克明i,2,金 莹1,康林萍1 ...查看


  • 炼钢基本原理
  • 第一章.炼钢基本原理 1.炼钢基本任务    钢与铁的区别 炼钢的基本任务 主要的炼钢工序 钢铁生产工艺流程 炼钢是将铁水(生铁).废钢等加热. 熔化,通过化学反应去除铁液中的 有害杂质,配加合金并浇铸成半成 品-铸坯的生产过程. 2 ...查看


热门内容