Development of an Opto fluidic Microsystem Dedicated to Chemical Analysis in a Nuclear Environment Procedia Chemistry 21 ( 2016 ) 453 – 460 1876 6196 © 2016 The Authors Published by Elsevier B V This[.]
Available online at www.sciencedirect.com ScienceDirect Procedia Chemistry 21 (2016) 453 – 460 WK,QWHUQDWLRQDO$7$/$17(&RQIHUHQFHRQ1XFOHDU&KHPLVWU\IRU6XVWDLQDEOH)XHO&\FOHV 'HYHORSPHQWRIDQRSWRIOXLGLFPLFURV\VWHPGHGLFDWHGWRFKHPLFDO DQDO\VLVLQDQXFOHDUHQYLURQPHQW )DELHQ*HRIIUD\D7LPRWKHH$OOHQHWE)DEULFH&DQWRD /DXUHQW&RXVWRQD'DYLGH%XFFLE (OVD-DUGLQLHUDE-HDQ(PPDQXHO%URTXLQE a CEA, Nuclear Energy Division, RadioChemistry & Processes Department, SERA/LAMM, F-30207 Bagnols-sur-Cèze, France IMEP-LaHC, Université de Grenoble Alpes, UMR 5130 CNRS, Minatec-Grenoble-INP, CS 50257, 38016 Grenoble, France b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© 2016 The Authors Published by Elsevier B.V This is an open access article under the CC BY-NC-ND license 7KH$XWKRUV3XEOLVKHGE\(OVHYLHU%9 (http://creativecommons.org/licenses/by-nc-nd/4.0/) 3HHUUHYLHZXQGHUUHVSRQVLELOLW\RIWKHRUJDQL]LQJFRPPLWWHHRI$7$/$17( Peer-review under responsibility of the organizing committee of ATALANTE 2016 Keywords:&KHPLFDODQDO\VLVPLFURV\VWHPPLQLDWXUL]DWLRQRSWRIOXLGLFVPLFURIOXLGLFLQWHJUDWHGRSWLFV ,QWURGXFWLRQ 6HYHUDO QXFOHDU HQHUJ\ SROLFLHV HQFRPSDVV WKH UHSURFHVVLQJ RI VSHQW QXFOHDU IXHO 61) DV D ZD\ WRZDUGV VXVWDLQDEOH FORVHG IXHO F\FOH 7KXV WKH 385(; SURFHVV LV ZLGHO\ HPSOR\HG LQ FRPPHUFLDO UHSURFHVVLQJ SODQWV &RUUHVSRQGLQJDXWKRU7HO E-mail address:)DEULFH&$172#FHDIU 1876-6196 © 2016 The Authors Published by Elsevier B.V This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/) Peer-review under responsibility of the organizing committee of ATALANTE 2016 doi:10.1016/j.proche.2016.10.063 454 Fabien Geoffray et al / Procedia Chemistry 21 (2016) 453 –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icrosystems for sensing 0LFURIOXLGLFVUHJDUGLQJ WUDQVSRUWDWLRQ DQGSURFHVVLQJRI OLTXLGVDPSOHV LQ PLFURVFDOHFKDQQHOVKDV LQGXFHG D UHYLYDO RI WKH PLFURDQDO\VLV LQ WKH V LQGHHG HQDEOLQJ WKH UHDOL]DWLRQ RI ODERQDFKLS RU PLFURWRWDO DQDO\VLV V\VWHPV $PRQJ WKH UHTXLUHG FRPSRQHQWV WKH GHWHFWLRQ LV HVVHQWLDO WR DFKLHYH TXDQWLWDWLYH PLFURDQDO\VLV DQG RSWLFDOPHWKRGVDUHWKXVUHOHYDQWIRUFRLQWHJUDWLRQRQWKHVDPHFKLSWRSHUIRUPUHPRWHDQDO\VHV,QWHJUDWHGRSWLFV LQWURGXFHGE\0LOOHULQWKHVSOD\VDPDMRUUROHLQWKHHIIRUWIRUDQ³RQFKLS´DSSURDFK7KHVHWHFKQRORJLHV WDNHEHQHILWRIPLFURIDEULFDWLRQWHFKQLTXHVWRLPSOHPHQWHLWKHURSWLFDORUIOXLGLFIXQFWLRQDOLWLHVRQSODQDUVXEVWUDWHV 7KHPHUJHRIPLFURIOXLGLFVZLWKLQWHJUDWHGRSWLFVOHDGVWRRSWRIOXLGLFGHYLFHV6HQVRUVUHO\LQJRQRSWRIOXLGLF SUHVHQWERWKFRPSDFWQHVVDQGPHFKDQLFDOUREXVWQHVVVLQFHWKHIXQFWLRQVDUHLQWHJUDWHGRQDVLQJOHFKLSZKLOHDOVR RIIHULQJ UHOLDELOLW\ WKDQNV WR VHOIDOLJQHG RSWLFV &RQVHTXHQWO\ RSWRIOXLGLFV KDYH IRXQG DSSOLFDWLRQV LQ FKHPLFDO DQDO\VLVDVUHSRUWHGLQUHYLHZSDSHUV 2.2 Previous works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c RI WKH DQDO\WH IOXLG WKURXJK WKH UHODWLRQVKLS D O H O c ZLWK H O WKH PRODU H[WLQFWLRQ FRHIILFLHQW WKDW FKDUDFWHUL]HV WKH DEVRUSWLRQ DFFRUGLQJ WR WKH ZDYHOHQJWK DQG ZKLFK LV VSHFLILF WR HDFK FKHPLFDO FRPSRXQG,QWKHFDVHRIWKHFRLQWHJUDWHGRSWRIOXLGLFVHQVRUGHVFULEHGSUHYLRXVO\RQO\DIUDFWLRQRIWKHJXLGHG OLJKW ZLOO HIIHFWLYHO\ LQWHUDFW ZLWK WKH IOXLGZKLFK OHDGV WR WKH LQWURGXFWLRQ RI DQ LQWHUDFWLRQIDFWRU * )LQDOO\ WKH DEVRUEDQFHVSHFWUXPLVH[SUHVVHGDV AO §I ORJ ăă L â I Ã áá v *H O cL ¹ 7KH LQWHUDFWLRQ IDFWRU LV D GLPHQVLRQOHVV TXDQWLW\ UDQJLQJ IURP WR ZKHUH XQLW\ FRUUHVSRQGV WR D IXOO LQWHUDFWLRQ EHWZHHQ WKH OLJKW VRXUFH EHDP DQG WKH DQDO\WH VROXWLRQ 7KLV LV REVHUYDEOH ZLWK FRPPHUFLDO VSHFWURSKRWRPHWHUZLWKDSDUDOOHOOLJKWEHDPFURVVLQJDVWDQGDUGFXYHWWH)RUWKHRSWRIOXLGLFVHQVRUWKHWKLFNQHVV 456 Fabien Geoffray et al / Procedia Chemistry 21 (2016) 453 – 460 d QF RI WKH QDQRFKDQQHO HQFRPSDVVHG ZLWKLQ WKH VORW ZDYHJXLGH PXVW EH FDUHIXOO\ VHW LQ RUGHU WR HQVXUH D JRRG LQWHUDFWLRQ IDFWRU ZKLOH EHLQJ WHFKQRORJLFDOO\ IHDVLEOH DQG HQDEOLQJ IOXLG IORZLQJ 7KH QDQRFKDQQHO WKLFNQHVV KDV EHHQWDLORUHGWKURXJKQXPHULFDOVLPXODWLRQVDQGIL[HGWR d QF QP7KLVQDQRVFDOHFKDQQHOIRUPVWKHFRUHRI WKH PLQLDWXUL]HG GHWHFWLRQ FHOO ZKRVH WHFKQRORJLFDO UHDOL]DWLRQ LV EULHIO\ SUHVHQWHG LQ WKH QH[W VHFWLRQ )URP D SUDFWLFDOSRLQWRIYLHZWKLVQDQRFKDQQHOLVFRQQHFWHGWRRXWHUHQYLURQPHQWWKRXJKPLFURVFDOHDFFHVVFKDQQHOV 3.2 Device fabrication 7KH VHQVRU LV PDGH RI %) JODVV IURP 6FKRWW 7KH QDQRFKDQQHO LV HQFDSVXODWHG LQ EHWZHHQ WZR JODVV VXEVWUDWHV VWDFNHG RQH RQ WRS RI WKH RWKHU DV LOOXVWUDWHG RQ )LJ 7KH SURFHVV IORZ KDV EHHQ IXOO\ GHVFULEHG LQ SUHYLRXVZRUNDQGLWFDQEDVLFDOO\EHGLYLGHGLQWRPDLQEXLOGLQJEORFNV x ,RQH[FKDQJHWHFKQRORJ\IRURSWLFDOZDYHJXLGHVIRUPDWLRQ x (WFKLQJWHFKQLTXHVIRUIOXLGLFFKDQQHOSDWWHUQLQJ x :DIHUERQGLQJ )LJ6HQVRUDUFKLWHFWXUHPDGHIURPWZRJODVVVXEVWUDWHV 'XULQJLRQH[FKDQJHWKHJODVVFRPSRVLWLRQLVORFDOO\PRGLILHGE\WKHVXEVWLWXWLRQRIWKHJODVVLRQVE\DQRWKHU LRQLFVSHFLHVIURPDQH[WHUQDOVRXUFH7KXVWKHUHIUDFWLYHLQGH[LVLQFUHDVHGHQVXULQJOLJKWJXLGLQJ7KHZDYHJXLGHV FDQHLWKHUEHFUHDWHGRQWKHZKROHJODVVVXEVWUDWHVXFKDVVXEVWUDWH$RQ)LJRUODWHUDOO\GHOLPLWHG$OOWKHGHWDLOV DERXWWKHRSWLFDOGHVLJQDQGJXLGLQJSURSHUWLHVKDYHEHHQUHSRUWHGLQSDVWZRUN 7KHQDQRFKDQQHOLVWKHQSDWWHUQHGLQWKHVXEVWUDWHZLWKSODQDUZDYHJXLGHE\GU\HWFKLQJ,QGXFWLYHO\&RXSOHG 3ODVPD 5HDFWLYH ,RQ (WFKLQJ ,&35,( WKLV WHFKQLTXH EHLQJ XVHG IRU VKDOORZ FKDQQHOV 6LQFH ,&35,( LV DQ DQLVRWURSLFHWFKLQJWHFKQLTXHWKHREWDLQHGFKDQQHOH[KLELWVDUHFWDQJXODUSURILOHZKRVHGHSWKLVFRQWUROOHGXVLQJD SURILORPHWHU DQG HVWLPDWHG WR d QF r QP $FFHVV PLFURFKDQQHOV DUH DOVR HWFKHG LQ WKH VDPH VXEVWUDWH ZLWK FRQFHQWUDWHG K\GURIOXRULF DFLG 7KLV LVRWURSLF ZHW HWFKLQJ DOORZV GHHSHU FKDQQHOV IRUPDWLRQ ZLWK VHPLFLUFXODU SURILOHVDVGHSLFWHGRQ)LJIRUWKHPGHHSDQGPZLGHFKDQQHOV )LJ&URVVVHFWLRQDOSKRWRJUDSKRIHQFDSVXODWHGDFFHVVPLFURFKDQQHO 457 Fabien Geoffray et al / Procedia Chemistry 21 (2016) 453 –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xperimental setup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abien Geoffray et al / Procedia Chemistry 21 (2016) 453 – 460 FDUERQDWHELFDUERQDWHEXIIHUVROXWLRQ±S+ LQRXUH[SHULPHQWDOFRQGLWLRQV±FRQWDLQLQJ0RIIOXRUHVFHLQ KDVEHHQXVHGIRUWKHIORZLQYHVWLJDWLRQVLQWKHQDQRFKDQQHO7KHIOXRUHVFHLQLVH[FLWHGZLWKD O QPDUJRQ ODVHU DQG IOXRUHVFHQFH VLJQDO PHDVXUHG ZLWK D &&' FDPHUD 6969,67(. HFR&9*( &RQVLGHULQJ WKH WKLFNQHVV RI WKH QDQRFKDQQHO WKH FRQIRFDO SLQKROH LV NHSW ZLGH RSHQ DQG KLJK JDLQ LV DSSOLHG 7KH QDQRVFDOH FKDQQHO LV ULQVHG ZLWK GHLRQL]HG ZDWHU %RWK UHSHDWDELOLW\ DQG UHSURGXFLELOLW\ RI WKH QDQRFKDQQHO ILOOLQJ DUH WKHQ GLVFXVVHG 4.2 Repeatability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± WKLV GXUDWLRQ EHLQJ HPSLULFDOO\ HVWLPDWHG±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abien Geoffray et al / Procedia Chemistry 21 (2016) 453 – 460 4.3 Reproducibility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±QRWGLVSOD\HGRQWKHJUDSKVIRUWKHVDNHRIFODULW\7KHVHPHDVXUHPHQWVKHQFHYDOLGDWH WKHWHFKQRORJLFDOUHDOL]DWLRQRIWKHRSWRIOXLGLFVHQVRU )LJ)LOOLQJWLPHPHDVXUHPHQWVFRQGXFWHGRQWZRGLIIHUHQWFKLSV &RQFOXVLRQ 7KHYROXPHUHGXFWLRQRIIHUHGE\DPLFURIOXLGLFDSSURDFKLVRISDUWLFXODULQWHUHVWIRUFKHPLFDODQDO\VLVLQQXFOHDU HQYLURQPHQWVLQFHWKHUDGLDWLRQGHFUHDVHVDFFRUGLQJO\0RUHRYHUWKHFRPELQDWLRQZLWKLQWHJUDWHGRSWLFVOHDGVWRWKH FRQFHSWLRQRIRSWRIOXLGLFVHQVRUVRQDVLQJOHJODVVFKLS7KHFKRVHQDUFKLWHFWXUHIRUDEVRUSWLRPHWULFPHDVXUHPHQWV 460 Fabien Geoffray et al / Procedia Chemistry 21 (2016) 453 –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|JVHOLXV36SHQWQXFOHDUIXHOSROLFLHVLQKLVWRULFDOSHUVSHFWLYH$QLQWHUQDWLRQDOFRPSDULVRQEnergy Policy 6LOYHULR/%GH4XHLUR]/DPDV:$QDQDO\VLVRIGHYHORSPHQWDQGUHVHDUFKRQVSHQWQXFOHDUIXHOUHSURFHVVLQJEnergy Policy ,QWHUQDWLRQDO $WRPLF (QHUJ\ $JHQF\ ,$($ 'HYHORSPHQW RI DGYDQFHG UHSURFHVVLQJ WHFKQRORJLHV ,Q 3URFHHGLQJV RI WKH QG JHQHUDO FRQIHUHQFH RI PHPEHU VWDWHV 9LHQQD $YDLODEOH DW KWWSVZZZLDHDRUJ$ERXW3ROLF\*&*&*&,QI'RFXPHQWV(QJOLVK JFLQIDWWBHQSGI! %DXPJlUWQHU)(UWHO'7KHPRGHUQ385(;SURFHVVDQGLWVDQDO\WLFDOUHTXLUHPHQWVJ Radioanal Chem. %U\DQ6$/HYLWVNDLD7*et al6SHFWURVFRSLFPRQLWRULQJRIVSHQWQXFOHDUIXHOUHSURFHVVLQJVWUHDPVDQHYDOXDWLRQRIVSHQWIXHOVROXWLRQVvia 5DPDQYLVLEOHDQGQHDULQIUDUHGVSHFWURVFRS\Radiochim Acta -DQVVHQV0DHQKRXW * %X\VW - et al 5HGXFLQJ WKH UDGLRDFWLYH GRVH RI OLTXLG VDPSOHV WDNHQ IURP UHSURFHVVLQJ SODQW YHVVHOV E\ YROXPH UHGXFWLRQNucl Eng Des. -DQVVHQV0DHQKRXW*1XFLIRUD6)HDVLELOLW\VWXG\RIDPLFURV\VWHPWRDQDO\VHUDGLRDFWLYHVROXWLRQVNucl Eng Des. 9HOWNDPS'-1HZ3ODWIRUPIRU6DPSOLQJDQG6HQVRU,QLWLDWLYH1H66,,Q.RFN099DQGHQ%XVVFKH.0&KULVPDQ5:(GLWRUV Micro Instrumentation: for High Throughput Experimentation and Process Intensification – a Tool for PAT:HLQKHLP:LOH\9&+S -DUGLQLHU(%XFFL'HWDO*ODVVLQWHJUDWHGQDQRFKDQQHOZDYHJXLGHIRUFRQFHQWUDWLRQPHDVXUHPHQWV,Q3URF63,(2372Integrated Optics: Devices, Materials, and Technologies XVII6DQ)UDQFLVFR,QWHUQDWLRQDO6RFLHW\IRU2SWLFVDQG3KRWRQLFVSS/ +LOOLV027KH+LVWRU\RI0LFURDQDO\VLVJ Chem Educ. :KLWHVLGHV*07KHRULJLQVDQGWKHIXWXUHRIPLFURIOXLGLFVNature 0DQ]$*UDEHU1:LGPHU+00LQLDWXUL]HG7RWDO&KHPLFDO$QDO\VLV6\VWHPVD1RYHO&RQFHSWIRU&KHPLFDO6HQVLQJSensor Actuat BChem. /LP