MIKROANALIZA FAZ V JEKLIH IN NIKLJEVIH ZLITINAH S POVRATNO SIPANIMI ELEKTRONI V VRSTI^NEM ELEKKTRONSKEM MIKROSKOPU
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1 ISSN KZLTET 32(5)379(1998) H. Kaker, V. Marikovi}: Mikroaaliza faz v jeklih... MIKROANALIZA FAZ V JEKLIH IN NIKLJEVIH ZLITINAH S POVRATNO SIPANIMI ELEKTRONI V VRSTI^NEM ELEKKTRONSKEM MIKROSKOPU PHASE MICROANALYSIS IN STEELS AND NICKEL ALLOYS BY BACKSCATTERED ELECTRONS IN THE SCANNING ELECTRON MICROSCOPE HENRIK KAKER 1, V. MARINKOVI] 2 1 S@-Metal Rave, d.o.o., SEM-EDS Laboratorij, Koro{ka cesta 14, 2390 Rave a Koro{kem 2 Istitut Jo ef [tefa, 1000 Ljubljaa Prejem rokopisa - received: ; sprejem za objavo - accepted for publicatio: V ~laku obravavamo uporabo povrato sipaih elektroov v vrsti~em elektroskem mikroskopu za mikroaalizo biarih i psevdo-biarih faz v jeklih i ikljevih zlitiah. Z meritvijo koeficieta povratega sipaja i v kombiaciji z rezultati mikroaalize EDS je mo o idetificirati faze z lahkimi elemeti, kot so karbidi, karboitridi, itridi i boridi, ter ugotoviti jihovo sestavo. Klju~e besede: vrsti~i elektroski mikroskop, povrato sipai elektroi, koeficiet povratega sipaja, mikroaaliza, faze v jeklih i ikljevih zlitiah The use of backscattered electros i the scaig electro microscope for microaalysis of biary ad pseudo-biary phases i steels ad ickel alloys is described. By measuremets of backscatterig coefficiets i combiatio with the EDS aalysis the presece of light elemets ca be detected i phases like carbides, carboitrides, itrides ad borides. Key words: scaig electro microscope, backscattered electros, backscatterig coefficiets, microaalysis, phases i steels ad ickel alloys 1 UVOD Osova za aalizo kemijske sestave materialov z uporabo povrato sipaih elektroov (PSE) v vrsti~em elektroskem mikroskopu (SEM) 1-3 je mooto porast koeficieta PSE z atomskim {tevilom elemetov, i sicer je ta porast za la je elemete (Z < 30) ekoliko hitrej{i kot za te je (slika 1). Taka odvisost koeficieta PSE, ki je defiira z razmerjem med tokom PSE i tokom vpadih elektroov, se lahko uporabi za idetifikacijo i kvatitativo aalizo biarih i psevdo - biarih faz 3. Aaliza s PSE e more adomestiti retgeske mikroaalize z eergijsko disperzivim (EDS) spektrometrom, ampak je predvsem dopolila metoda k aalizi EDS faz z lahkimi elemeti z atomskimi {tevili pod 11, ki jih z EDS-detektorji z berilijevim okom i mogo~e aalizirati zaradi absorpcije retgeske svetlobe v oku detektorja. Kombiacija EDS-aalize i aalize s PSE omogo~a idetifikacijo i dolo~itev sestave faz, kot so karbidi, karboitridi, itridi, boridi i oksidi, vedar pa je kvatitativa aaliza omejea a biare i psevdo-biare faze. Poleg hitre kvalitative i kvatitative aalize teh faz omogo~a aaliza s PSE tudi meritve debelie delcev v matricah ter debelie i sestave povr{iskih takih plasti. V vseh omejeih primerih je za aalize potrebo pozavaje odvisosti koeficietov PSE od atomskega {tevila. V literaturi so podai razi aaliti~i modeli pa tudi empiri~e ea~be za izra~u koeficietov PSE 4. Za teoreti~e izra~ue je zaradi arave sipalega procesa posebej primera metoda simulacije Mote Carlo (MC) 5. V ~laku so prikazai rezultati MC-izra~uov globi i premerov iterakcijskih volumov v zvezi z aalizo problematiko, specifi~osti meritev relativih koeficietov PSE ter postopek i rezultati aalize ekaterih faz, ki vsebujejo lahke elemete. 2 SIMULACIJA MONTE CARLO Iterakcije elektroov z atomi vzorca so zelo komplekse arave. Prede elektro izgubi svojo eergijo ali izstopi iz vzorca, do ivi moge elasti~e i eelasti~e trke. Za obravavo iterakcij vpadega elektroa se uporablja metoda Mote Carlo 5, s katero simuliramo tridimezioale trajektorije vpadega elektroa v vzorcu. Reali curek elektroov je sestavlje iz mogih elektroov, zato moramo v izra~uu simulirati veliko {tevilo elektroov. Simulacija Mote Carlo se v elektroski mikroskopiji uporablja za dolo~itev velikosti primarega iterakcijskega voluma, kote i eergijske porazdelitve i iterakcijskih volumov povrato sipaih i sekudarih elektroov, izra~u koeficietov trasmisije, porazdelitve retgeskega sigala z globio i simulacijo katode lumiiscece. Programi za MC-simulacije so fleksibili glede defiiraja istrumetalih parametrov i relevatih karakteristik vzorca 6, zato je metoda pomembe pripomo~ek pri aalizi meritev povratega sipaja elektroov. Uporaba MC simulacije KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5 379
2 V tabeli 1 so podai tako izra~uai premeri i globie iterakcijskih volumov v Fe za primare i PS elektroe ter za karakteristi~o retgesko sevaje FeK α v odvisosti od eergije pri pravokotem vpadu elektroov. Za 25 kev elektroe sta iterakcijska voluma za primare i PS-elektroe prikazaa tudi grafi~o a sliki 2. Izra~ui so tudi pokazali, da 90% PSE izstopa s povr{ie, katere premer je okrog 30% dosega elektroov 7. Iz rezultatov v tabeli izhaja, da so izstopi volumi za PSE maj{i od ustrezih vredosti za FeK α, oziroma, da je prostorska lo~ljivost 7 aalize s PSE bolj{a kot pri retgeski mikroaalizi. Slika 1: Odvisost koeficieta PSE od atomskega {tevila vzorca 12 Figure 1: Variatio of backscattered electro coefficiet with atomic umber 12 je {e posebej epogre{ljiva v primerih, ko so laterale dimezije aaliziraih podro~ij, pr. izlo~kov v matricah, primerljive s premeri iterakcijskih volumov elektroov. Za simulacijo sipaja elektroov z metodo Mote Carlo so v rabi razli~i modeli, ki se med seboj razlikujejo po a~iu opisa trajektorij elektroov v vzorcu. Za izra~ue, potrebe pri aalizih meritvah, smo uporabili model ve~kratega sipaja 6, ki je primere za opis karakteristik PSE v SEM v eergijskem obmo~ju med 5 i 40 kev. Zaemaritev eelasti~ega sipaja v modelu povzro~i le majho apako, zelo pa poeostavi i za pet- do osem-krat skraj{a izra~ue v primerjavi z modelom ekratega sipaja 6. Za uporabljei model smo apisali ra~uali{ki program v programskem jeziku Power Basic verzija 2.0 (Spectra Publishig, ZDA) za IBM PC ali kompatibili ra~ualik. Pri izra~uih smo simulirali od 1000 do 5000 trajektorij elektroov a ra~ualiku IBM PC s 75 MHz Petium-procesorjem. Potrebe ~as za simulacijo 5000 elektroov je okrog 6 miut. Pri simulaciji 5000 elektroov je relativa apaka rezultata simulacije 1,4%. Slika 2: Iterakcijski volume za primare elektroe i PSE za Fe pri 25 kev i pravokotem vpadu elektroov (simulacija 100 elektroov) Figure 2: Iteractio volume of primary electros ad backscattered electros at 25 kev i Fe, ormal icidece, (simulatio of 100 electros) Tabela 1: Izra~uae dimezije iterakcijskih volumov v Fe v odvisosti od eergije Table 1: Depedace of eergy ad calculated dimesios of iteractio volumes i Fe Eergija Eo Primari elektroi Fe Kα Povrato sipai elektroi (kev) premer globia premer globia premer globia 1 0,06 0, ,04 0,02 5 0,22 0, ,14 0, ,67 0,54 0,61 0,49 0,41 0, ,37 1,12 1,26 0,99 0,93 0, ,22 1,84 2,20 1,80 1,46 0, ,36 2,67 3,25 2,63 2,07 0, ,54 3,66 4,51 3,58 3,54 1, ,30 4,83 6,26 4,72 4,08 1, ,57 6,10 7,36 5,90 5,84 2,25 3 MERITVE RELATIVNEGA KOEFICIENTA POVRATNEGA SIPANJA Za detekcijo PSE v SEM se uporabljajo polprevodi{ki detektorji 8, ki so avado izdelai kot simetri~i elemeti s cetralo odprtio i omogo~ajo detekcijo PSE z eergijami okrog 1 kev i lo~ljivostjo 0,2 atomskega {tevila. Za meritve koeficietov PSE s polprevodi{kim detektorjem je treba pozati karakteristike detektorja (spodji prag detekcije, izkoristek) ter kote i eergijske porazdelitve PSE, ki pa so odvise od sestave vzorca. Ker ti parametri ve~ioma iso pozai, so za aalize meritve pri uporabi polprevodi{kega detektorja primere le meritve relativih koeficietov PSE. Ta je defiira kot razmerje med sigalom vzorca i stadarda. Meritev je uspe{a pri pogoju, da so vse astavitve a SEM kostate za vzorec i stadard. Ker a meritve relativih koeficietov vpliva ve~ eksperimetalih faktorjev, je treba zvezo med koeficieti PSE i Z dolo~iti eksperimetalo s primero kalibracijo. Glavi faktorji, ki vplivajo a meritev relativega koeficieta PSE, so: a) Geometrija vzorec - detektor: Razdalja med vzorcem i detektorjem je kriti~a, ker dolo~a prostorski kot detekcije PSE. Pri uporabi polprevodi{kega detektorja, ame{~eega pod polove ~evlje objektive le~e 380 KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5
3 (slika 3), je razdalja med vzorcem i detektorjem zelo ata~o astavljiva z Z - goiometrsko stopjo. b) Meritev sigala: Oja~ei apetosti sigal iz detektorja PSE se vodi a SEM moitor i se lahko uporabi za meritev relativega koeficieta PSE. Vedar je treba v tem primeru zagotoviti kostatost preve~ parametrov, kot so razdalja vzorec - detektor, tok curka elektroov i astavitve a oja~evaliku. Zaradi tega smo vse meritve sigala opravili eposredo a izhodu detektorja z merilikom toka. c) Tok curka i odziv detektorja: Ker je merjei sigal sorazmere toku curka, so meritve relativih koeficietov PSE reproducibile samo, ~e je tok curka med meritvijo kostate a vzorcu i stadardu. Tok curka smo merili s Faradayevo kletko, vgrajeo v osilec vzorca. Preizku{aje odziva detektorja s serijo meritev a bakrovem stadardu v obmo~ju med 6 i 30 kev je pokazalo, da je v obmo~ju ad 13 kev odziv detektorja lieare (slika 4). d) Topografija vzorca: Sigal PSE je odvise od variacij topografije vzorca 2. Prispevek zaradi topografije vzorca se elimiira z zelo skrbo pripravo vzorcev i ko~im polirajem z 1/4 µm diamato pasto. Meritev hrapavosti poliraega vzorca je bila opravljea z merilikom Pathomether 5SP v metrolo{kem laboratoriju firme S@-STO Rave, d.o.o. Za polirai vzorec jekla OCR 12 je povpre~a vredost petih meritev R a = 0,03 µm (aritmeti~o sredje odstopaje od izmerjeega profila hrapavosti). e) Kotamiacija povr{ie vzorca: V mogih primerih a sve e poliraih vzorcih zelo hitro zraste a zraku oksida plast 2 debelie do 5 m. Dodata plast kotamiacije se lahko abere a povr{ii vzorca v SEM kot posledica iterakcije med curkom elektroov i ogljikovodikovimi kompoetami preostale atmosfere. Vpliv kotamiacije se lahko ugotovi z opazovajem spremembe sigala PSE v odvisosti od ~asa. V 200 sekudah se merjei sigal PSE od bakrovega stadarda, obsevaega z 20 kev curkom, zmaj{a za 0,5%. Ker pa je avado ~as aalize kraj{i od 5 sekud, je vpliv kotamiacije zaemarljiv. 4 EKSPERIMENTALNO DELO 4.1 Priprava vzorcev Uporabljei stadardi (~istota 99,9 mas.%) elemetov za pripravo kalibracijske krivulje, vzorci jekel i ikljevih zliti so bili kemi~o aalizirai v kemijskem laboratoriju firme S@ - Metal Rave, d.o.o. z retgeskim kvatometrom firme ARL. Vse vzorce smo skupaj z bakrovim stadardom (~istota 99,9 mas.%) zalili v hlado strjevalo maso i jih pripravili kot je potrebo za opazovaje v mikroskopu. Vse vzorce smo pred meritvijo kratek ~as odpolirali z 1/4 µm diamato pasto, da smo odstraili evetualo oksido plast i jih takoj vstavili v SEM. Sestava preiskovaih vzorcev je podaa v tabeli 2, jihove ozake so v skladu z razvrstitvijo jekel firme S@ - Metal Rave, d.o.o. Tabela 2: Kemijska sestava vzorcev (v mas.%) Table 2: Chemical compostio of samples (i weight %) C 45 OC120 OCR12 OCR12VM PK 924 N80A C 0,44 1,05 2,02 1,56 0,08 0,03 Al - - 0,019 0,042 0,69 1,26 Si 0,24 0,15 0,25 0,24 0,87 0,19 P 0,022 0,017 0,021 0,034 0,025 - S 0,073 0,020 0,08 0,020 0,018 0,002 Ti ,017-2,28 V - 0,02-0, Cr 0,23 0,08 11,72 11,58 17,42 19,40 M 0,48 0,22 0,32 1,65 0,57 0,07 Fe 97,98 98,19 85,16 81,26 79,92 1,21 Co , Ni 0,23 0,02 0,21 0,11 0,13 75,55 Cu 0,27 0,23 0,12 0,21 0,20 0,01 Mo 0,03-0,08 2,11 0,08 - W , Slika 3: Shema meritve relativega koeficieta PSE Figure 3: Backscattered coefficiet measuremet arragemet Slika 4: Izhod iz detektorja v odvisosti od eergije elektroskega curka Figure 4: Variatio of detector output sigal with the eergy of electro beam KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5 381
4 4.2 Meritve Vse meritve smo opravili z istrumetom SEM JEOL 35 - CF. Relative koeficiete PSE smo merili s polprevodi{kim detektorjem JEOL 35 - BEI, tokove pa z merilikom toka firme K.E. Developmets 9 z merilim obmo~jem do A (to~ost +/- 2% v obmo~ju do A i +/- 5% v obmo~ju do A). Pri vseh meritvah smo kot stadard uporabil baker. Zaradi te av, omejeih v to~ki 3.b, smo sigal PSE merili eposredo a izhodu detektorja PSE. Vse aalize smo opravili a 5 aklju~o izbraih mestih vzorcev z metodo to~kove aalize pri pravokotem vpadu elektroov i 10 mm razdalji vzorec - detektor ter v aalizem ~asu 3 s. Pospe{evale apetosti pri meritvah so bile izbrae v skladu z velikostjo aaliziraih delcev, tako da i pri{lo do prodiraja elektroov v matrico i lateralega sipaja elekroov. Premer curka elektroov se v SEM meri z liijskim rastrirajem preko roba zlomljee rezie Si i meritvijo sigala presevih elektroov. Ker SEM JEOL JSM 35 - CF i opremlje z detektorjem presevih elektroov, smo premer curka elektroov oceil z uporabo Smithovega 10 diagrama. Za pospe{evale apetosti med 10 i 30 kev, tokove 10-8 do A i volframovo itko je ocejei premer curka elektroov med 10 i 200 m i je bistveo maj{i od premera aaliziraih faz. Za aalize EDS smo uporabili eergijski spektrometer EDAX 9100/40, za retgesko uklosko aalizo (XRD) pa strukturi retge Siemes Kristalloflex 4. SEM-slike so bile posete z uporabo povrato sipaih elektroov i prikazujejo Z-kotrast, to je kotrast zaradi razlik v popre~em atomskem {tevilu prisotih faz. 4.3 Kalibracija Za kalibracijo smo uporabili {tevile vzorce ~istih elemetov, ki smo jih aalizirali pri 15, 20 i 25 kev i pravokotem vpadu elektroov, 10 mm razdalji vzorec - detektor i kostatem toku curka. Vse vredosti izmerjeih sigalov so ormalizirae glede a vredost, dobljeo a bakrovem stadardu. Z metodo ajmaj{ih kvadratov smo dobil ea~be za odvisost relativega koeficieta PSE od atomskega {tevila pri 15, 20 i 25 kev za obmo~je od Z = 6 do Z = 83: η r = a+b.10-2.z+c.10-4.z 2 +d.10-6.z 3, (1) kjer je η r relativi koeficiet PSE i Z atomsko {tevilo. Vredosti koeficietov a, b, c i d za vse tri eergije so podae v tabeli 3. Tabela 3: Koeficieti a, b, c i d v ea~bi (3) Table 3: Coefficiets a, b, c i equatio (3) kev a b c 15-0,220 6,325-9, ,223 6,383-9, ,223 6,385-9,237 5 ANALIZA FAZ, KI VSEBUJEJO LAHKE ELEMENTE S KOMBINACIJO ANALIZE S PSE IN EDS 5.1 Opis postopka Pri aalizi s PSE ugotovimo povpre~o atomsko {tevilo faze Z p(pse) iz izmerjeega relativega koeficieta PSE i ustreze kalibracijske krivulje. V primeru, da je razlika vredosti povpre~ih atomskih {tevil dveh faz maj{a od lo~ile zmo osti polprevodi{kega detektorja, (po podatkih iz literature 8 je Z P 0,2) ju samo s PSE i mogo~e razlikovati. Vedar pa ju v takem primeru, kot pr: AlN z Z p = 10,9 i SiO 2 z Z p = 10,8 v SEM lahko idetificiramo z EDS. V splo{em lahko sestavo faz z lahkimi elemeti ugotovimo s kombiacijo podatkov EDS-aalize i aalize s PSE. Pri tem je strategija aalize asledja. Aalizi s PSE i EDS dajeta podatke o povpre~em atomskem {tevilu faze, prisotih elemetih i jihovi koli~ii oziroma relativih dele ih teh elemetov. Povpre~o atomsko {tevilo faze Z p(eds) izra~uamo iz podatkov EDS-aalize i je po ea~bi Daguya i Quivya 2 : Z = 2 α i Z i (2) α i Z i kjer je α i - {tevilo atomov i Z i - atomsko {tevilo i - te kompoete v fazi. V primerih, ko je Z p(eds) P Z p(pse), faza e vsebuje lahkih elemetov, Z p(eds) ve~ji od Z p(pse) pa pomei, da aaliziraa faza vsebuje lahke elemete. Iz tako dobljeih podatkov ato sestavo faze izra~uamo z uporabo Castaigove ea~be 4, po kateri je koeficiet PSE ve~kompoetega vzorca η p eak vsoti produktov masih kocetracij elemetov c i, ki sestavljajo vzorec, i jihovih koeficietov PSE η i: η p = c i η i, c i = 1 (3) i ki omogo~a dolo~itev sestave biarih i psevdobiarih faz. 5.2 Rezultati aalize faz v jeklih i ikljevih zlitiah Uporabost PSE za aalizo faz, ki vsebujejo lahke elemete, smo preizkusili a sulfidih i oksidih vklju~kih ter a karbidu i karboitridu v vzorcih orodih i erjavih jeklih ter ikljevih zliti. Za aalizo so bili izbrai le delci faz s premeri, ve~jimi od premerov iterakcijskih obmo~ij izra~uaih z Mote Carlo simulacijo, ki so podai v tabeli 4a. Sestavo faz pri EDS i PSE-aalizi smo izra~uali po metodi ZAF (program CITZAF 11 ) i re{itvijo ea~be (3), kot je opisao v prej{ji to~ki. 382 KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5
5 Tabela 4a: Rezultati izra~ua Mote Carlo vzbujevalih volumov za aalizirae faze Table 4a: Results of Mote Carlo calculatio of iteractio volumes for the phases Aaliziraa faza Vzorec Posp. apetost (kv) Premer faze Vzbujevali volume primarih elektroov Vzbujevali volume povrato sipaih elektroov premer globia premer globia MS CK ,5-35 5,58 2,58 4,58 0,83 Fe 3C OC ,4-2 0,98 0,40 0,64 0,15 M 7C 3 OCR ,45 1,50 2,45 0,55 SiO 2 OCR 12VM ,23 3,80 4,94 1,29 Al 2O 3 PK ,64 2,35 3,35 0,71 Ti(C,N) N80A ,57 2,14 3,07 0,78 Tabela 4b: Izra~uai i izmerjei relativi koeficieti PSE i povpre~a atomska {tevila aaliziraih faz Table 4b: Calculated ad measured relative backscattered electro coefficiets ad averaged atomic umbers of aalyzed phases Aaliziraa faza Relativi koeficiet PSE (MC) η r Relativi koeficiet PSE (izmerje η r) Atomsko {tevilo dobljeo s PSE Z p Atomsko {tevilo dobljeo s EDS Z p EDS sestava v mas.% MS 0,78 0,76 21,10 21,51 38,8%S, 61,2%M Fe 3C 0,93 0,86 24, %Fe M 7C 3 0,88 0,81 22,86 24,90 55,1%Cr, 44,9%Fe SiO 2 0,39 0,37 9, %Si Al 2O 3 0,38 0,36 9, %Al Ti(C,N) 0,59 0,60 16, %Ti Tabela 4c: Korigirae sestave faz Table 4c: Corrected phase compositio Aaliziraa faza Korigiraa sestava v mas.% Korigiraa sestava v mas.% Korigirao atomsko {tevilo Z P MS 39,8% S, 60,2% M 52,6% S, 47,4% M 21,42 Fe 3C 4,7% C, 95,3% Fe 18,6% C, 81,4% Fe 25,06 M 7C 3 8,7%C,50,3%Cr,40,9%Fe 29,8%C,39,1%Cr,30,3%Fe 23,3 SiO 3 49,1% O, 50,9% Si 63,4% O, 36,6% Si 11,05 Al 2O 3 44,2% O, 55,8% Al 57,8% O, 42,2% Al 10,79 Ti(C,N) 13,9%C,16,1%N,70,0%Ti 30,7%C,30,5%N,38,8%Ti 17,36 Slika 5: MS vklju~ki, Z-kotrast i EDS-spekter Figure 5: MS iclusios, Z-cotrast ad EDS specter KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5 383
6 Slika 6: Fe 3 C faze, Z-kotrast i EDS-spekter Figure 6: Fe 3 C phases, Z-cotrast ad EDS specter Slika 7: M 7 C 3 faze, Z-kotrast i EDS spekter Figure 7: M 7 C 3 phases, Z-cotrast ad EDS specter V tabeli 4a so zbrai podatki o pospe{evalih apetostih, obmo~jih velikosti delcev aaliziraih faz i izra~uai premeri i globie iterakcijskih volumov za primare i povrato sipae elektroe. V tabeli 4b so primerjai izra~uai izmerjei relativi koeficieti PSE i popre~a atomska {tevila iz PSE i iz EDS-aaliz ter sestava faz, dolo~ea z EDS-aalizo. Korigirae vredosti sestav v masih i atomskih odstotkih i korigiraa atomska {tevila vsebuje tabela 4c. Relative apake aalize smo izra~uali po ea~bi: r = C KA C PSE,EDS 100, (4) C KA kjer je r - relativa apaka aalize, C PSE,EDS - masa kocetracija elemeta, ugotovljea s PSE ali EDS, i C KA - masa kocetracija elemeta, dolo~ea s kemijsko aalizo (KA). Delci i EDS-spektri ter retgeograma so prikazai a slikah 5 do 9. Rezultat PSE-aalize MS v jeklu CK45 se precej dobro ujema z rezultati EDS-aalize i stehiometri~o sestavo (36,8 mas.% S i 63,2 mas.% M). Relativa apaka aalize, izra~uaa po ea~bi (4), je v primerjavi s Slika 8: Retgeogram karbide faze M 7 C 3 v jeklu OCR12 Figure 8: X-Ray diffractio spectrum of M 7 C 3 phase i steel OCR12 stehiometri~o sestavo: 8,1 mas.% za S i 4,9 mas.% za M. Sestava faze se tudi dobro ujema z objavljeim eksperimetalim podatkom Schwaaba 12 (39,8 mas.% S i 60,2 mas.% M). Sestava faze Fe 3C v jeklu OC120 se slabo ujema s stehiometri~o sestavo (6,7 mas.% C i 93,3 mas.% Fe). Relativa apaka aalize je v primerjavi s stehiometri~o sestavo: 29,8 mas.% za C i 2,1 mas.% za Fe. Russ 13 je v jeklu s krogli~im perlitom dobil sestavo Fe 3C (aali- 384 KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5
7 Slika 9: Ti(C, N) faza, Z-kotrast i EDS spekter Figure 9: Ti(C, N) phase, Z-cotrast ad EDS specter zirao z EDS za detekcijo lahkih elemetov): 6,50 mas.% C i 93,02 mas.% Fe s to~ostjo +/- 10%. Izra~uaa empiri~a formula karbide faze (Cr 4,02Fe 3,03)C 3,00 v jeklu OCR12 (M/C = 2,35) se dobro ujema z rezultatom XRD aalize (M/C = 2,33). Sestava faze SiO 2 v jeklu OCR12VM se dobro ujema s stehiometri~o sestavo (46,7 mas.% O i 53,3 mas.% Si). Relativa apaka aalize je v primerjavi s stehiometri~o sestavo: 5,1 mas.% za O i 4,5 mas.% za Si. Aaliziraa faza je glede a svojo velikost (dol ie do 200 i {irie do 50 µm) verjeto edogeega 14 izvora. Sestava faze Al 2O 3 v jeklu PK924 se dobro ujema s stehiometri~o sestavo (47,1 mas.% O i 52,9 mas.% Al). Relativa apaka aalize je v primerjavi s stehiometri~o sestavo: 1,3 mas.% za O i 5,5 mas.% za Al. V aaliziraem jeklu X10CrAl8 z vsebostjo 0,69 mas.% Al pride, po podatkih iz literature 14 do astaka ~iste faze Al 2O 3, kar je potrdila tudi aaliza z EDS i PSE. Sestava faze Ti(C, N) v zlitii N80A je izra~uaa s predpostavko, da je razmerje atomskih procetov ogljika i du{ika pribli o eako 50:50 i ustreza empiri~i formuli Ti 1,00(C 1,009,N 1,002). 6 SKLEPI Povpre~a relativa apaka aalize s PSE je +/- 7,6% i s stali{~a EDS mikroaalize ustreza rezultatom semi kvatitative mikroaalize 15 (+/- 10%). Odmiki rezultatov od dejaske sestave so lahko posledica eto~osti merile opreme (+/- 5%), estabilosti elektroskega toka (ve~ia SEM ima vgrajeih aprav za stabilizacijo toka) i karakteristik uporabljeega detektorja PSE (izkoristek). Poleg uporabosti za aalizo sovi z majhim atomskim {tevilom sta predosti metode bolj{a laterala lo~ljivost v primeri z retgesko mikroaalizo i relativo velika hitrost meritev, saj so podatki od vsake aalize to~ke zbrai v ekaj sekudah. 7 LITERATURA 1 Goldstei J. I., Jakowitz H., Practical Scaig Electro Microscopy, Pleum Press, (1977) 57-64, Ball M. D., McCartey D. G., Joural of Microscopy, 124 (1981) Heirich K. F. J., i Proceedigs of the 4th Iteratioal Cogress o X-Ray Optics ad Microaalysis, Paris 1965, Herma Press, Niedrig H., J. Appl. Phys., 53 (1982) 4, R15-R30 5 NBS SP 460, Use of Mote Carlo Calculatios i Electro Probe Microaalysis ad Scaig Electro Microscopy, Gaithersburg, 1975, Joy D. C., Mote Carlo Modelig for Electro Microscopy, Oxford Uiversity Press, 1995, Joy D. C., Joural of Microscopy, 136 (1984) Newbury D. E., Microbeam Aalysis , Sa Fracisco Press, 1981, Komerciali prospekt, Probe Curret Meter, K. E. Developmets td., Toft, Cambridge, CB3 9RL, Aglija 10 Smith K. C. A., Ph.D. Dissertatio, Uiversity of Cambrdige, Armstrog J. T., Program CITZAF, MAS software library, Uiversity of Michiga, USA, (FTP: freebie.egi.umich.edu) 12 Schwaab P., Practical Metallography, 23 (1986) Russ J. C., i Eergy Dispersive X-Ray Spectrometry, Ed. K. F. J. Heirich, NBS SP 604, Gaithersburg, USA, 1981, Kiesslig R., Lage N., No - metallic iclusios i steel, I, II, III, The Iro ad Steel Istitute Lodo, 1964, 1966, 1968, I: 1-92, II: 1-163, III: Russ J. C., Priciples of Edax Aalysis i the Electro Microscope, Edax Iteratioal Ic., 1978, 52 KOVINE, ZLITINE, TEHNOLOGIJE 32 (1998) 5 385
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