3D EDX Microanalysis by FIB-SEM: Enhancement of Elemental Quantification

 

'(';0LFURDQDO\VLVE\),%6(0(QKDQFHPHQWRI(OHPHQWDO4XDQWLILFDWLRQ

,QWHUGLVFLSOLQDU\ &HQWUH IRU (OHFWURQ 0LFURVFRS\ &,0( )HGHUDO ,QVWLWXWH RI 7HFKQRORJ\ RI /DXVDQQH(3)/6WDWLRQ&+/DXVDQQH6ZLW]HUODQG



6SDWLDOUHVROXWLRQRI(';DQDO\VLVRIEXONVDPSOHLVOLPLWHGE\LQWHUDFWLRQYROXPH7KLVYROXPHFDQ EH UHGXFHG ORZHULQJ DFFHOHUDWLRQ YROWDJH EXW WKH HQHUJ\ RI WKH HOHFWURQ EHDP QHHGV WR EH KLJK HQRXJK WR H[FLWH WKH FKDUDFWHULVWLF ;UD\V >@ 7KLV LV SDUWLFXODUO\ FULWLFDO LQ WKH FDVH RI VPDOO IHDWXUHV 7KH DFFXUDF\ RI DQ ('; DQDO\VLV GHFUHDVHV GUDVWLFDOO\ ZKHQ WKH LQWHUDFWLRQ YROXPH EHFRPHVELJJHUWKDQWKHIHDWXUHVL]H,QD),%6(0LWLVSRVVLEOHWRUHPRYHPDWHULDOVOLFHE\VOLFH DQGWRH[SORUHVRWKHVDPSOHLQWKHUGGLPHQVLRQ7KHVXEVHTXHQWVOLFHVUHYHDO WKLVZD\ZKDWWKH HOHFWURQVLQWKHLQWHUDFWLRQYROXPHKDYH³VHHQ´XQGHUWKHVXUIDFH7KHFKDUDFWHUL]DWLRQE\(';FDQ EHGRQHLQ'WKLVZD\>@8VLQJWKHDGGLWLRQDOVSDWLDOLQIRUPDWLRQVSHFWUDIURPWKH'VWDFNFDQ EHSRVWSURFHVVHGWRHQKDQFHWKHDFFXUDF\RIWKHTXDQWLILFDWLRQ,QWKLVZRUNDILUVWDSSURDFKWRVXFK SRVWSURFHVVLQJDOJRULWKPLVSURSRVHG 

&RQVLGHULQJ ' ('; DQDO\VLV WKH VWUXFWXUH EHORZ WKH VXUIDFH LV XQNQRZQ ZKLFK OHDGV WR DQ XQFHUWDLQW\RQWKHTXDQWLILHGFRPSRVLWLRQ+RZHYHULQVRPHVSHFLDOFDVHVDJRRGXQGHUVWDQGLQJRI WKHYDULDWLRQRIWKH;UD\LRQL]DWLRQ\LHOGZLWKGHSWKKDVOHGWRSURFHGXUHVWRSDUWLDOO\RYHUFRPHWKLV OLPLWDWLRQ>@)RUH[DPSOHLQWKHFDVHRIPXOWLOD\HUVWUDWLILHGVDPSOHVLWLVSRVVLEOHWRFDOFXODWH ERWKOD\HUWKLFNQHVVHVDQGFRPSRVLWLRQ3RXFKRXDQG3LFKRLUVXJJHVWHGDUHFXUVLYHSURFHGXUHEDVHG RQ WKHfr] FXUYH WKH ;UD\ JHQHUDWLRQ \LHOG ZLWK GHSWK >@ ,W QHHGHG ('; PHDVXUHPHQW DW VHYHUDO DFFHOHUDWLRQ YROWDJHV WR SUHYHQW FRQYHUJHQFH WR ORFDO PLQLPXP 6WDWKDP UHILQHG WKLV SURFHGXUHZLWKDQDOJRULWKPSUHGLFWLQJPHDVXUHPHQWFRQGLWLRQVWKDWFRQYHUJHWRDXQLTXHVROXWLRQ >@ :H SURSRVH WR DSSO\ WKLV SURFHGXUH WR ' ('; GDWD REWDLQHG ZLWK D ),%6(0 LQ RUGHU WR HQKDQFHHOHPHQWDOTXDQWLILFDWLRQ



7RDSSO\WKHVWUDWLILHGTXDQWLILFDWLRQSURFHGXUHWR'(';GDWDWKHIROORZLQJUHFXUVLYHUHODWLRQLV VXJJHVWHGDVLOOXVWUDWHGLQWKHILJXUH

&L$ f NUDWLRVL&L&L

:LWK&WKHFRQFHQWUDWLRQRIHOHPHQW$LQWKHLOD\HU),%VOLFHNUDWLRWKH;UD\LQWHQVLW\QRUPDOL]HG WR LQWHQVLW\ IURP  D VWDQGDUG DQGf WKH UHFXUUHQFH UHODWLRQ KHUH WKH VWUDWLILHG TXDQWLILFDWLRQ SURFHGXUH



7KLVDSSURDFKLVWHVWHGRQVHYHUDOVDPSOHVRIVLPSOHJHRPHWU\$QH[DPSOHIRUDVWUDWLILHGVDPSOHLV JLYHQ LQ ILJXUH  6LPXODWHG ;UD\ LQWHQVLWLHV DUH SORWWHG DV D IXQFWLRQ RI ] GLUHFWLRQ RI WKH ),% VOLFLQJSURJUHVV&RPSRVLWLRQVIRUHDFKRIWKHVHVOLFHVDUHFDOFXODWHGE\WKHVWDQGDUGTXDQWLILFDWLRQ SURFHGXUHDQGE\WKHDSSURDFKVXJJHVWHGKHUH$JHQHUDOHQKDQFHPHQWLVREVHUYHGIRUHDFKOD\HU $OOPDWHULDOVWHVWHGVKRZHGDQHQKDQFHPHQW%DVHGRQWKLVSURPLVLQJUHVXOWIXUWKHUWHVWVDUHGRQH RQVDPSOHVZLWKPRUHFRPSOH[FRPSRVLWLRQDQGJHRPHWU\LQRUGHUWRLPSURYHWKHDSSURDFKDQGWR SUHYHQWSLWIDOO   960

doi:10.1017/S1431927611005678 © Microscopy Society of America 2011Microsc. Microanal. 17 (Suppl 2), 2011

https://doi.org/10.1017/S1431927611005678





5HIHUHQFHV

>@ -,*ROGVWHLQHWDOScanning Electron Microscopy and X-ray Microanalysis3OHQXP1HZ <RUN

>@ 06FKDIIHUHWDOMicrochimica Acta >@ -3RXFKRXDQG)3LFKRLUScanning

>@ 3-6WDWKDPMaterials Science and Engineering >@ 7KLVUHVHDUFKLVVXSSRUWHGE\&DUO=HLVV607  ),*6FKHPDWLFSLFWXUHRIDPDWHULDOZLWKSKDVHV7KHYR[HOVRIWKH'(';DFTXLVLWLRQDUHWKH GDVKHGVTXDUHV(DFKYR[HOFRUUHVSRQGWRDKRUL]RQWDOVOLFHUHPRYHGE\WKHLRQEHDP   ),*6LPXODWHGVWUDWLILHGVDPSOH6HFWLRQVDUHPLOOHGDZD\E\WKHLRQEHDP7KHHOHFWURQEHDP KDV DQLQFLGHQW DQJOHRIGHJUHH .UDWLRVDV ZHOODVWKH FDOFXODWHGFRPSRVLWLRQVZVWDQGDUG TXDQWLILFDWLRQSURFHGXUHDUHGLVSOD\HG7KHRQHVODEHOHG³FRUU´DUHWKHFRPSRVLWLRQFDOFXODWHGZLWK WKHDSSURDFKVXJJHVWHGKHUH

Microsc. Microanal. 17 (Suppl 2), 2011 961

https://doi.org/10.1017/S1431927611005678