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Continuousflowsynthesisofphosphatebindingh-BN@magnetitehybrid
material
AhmedHusseinMohammedAl-antakia,XuanLuoa,b,AlexDuanc,RobertN.Lambc,ElaEroglud,WayneHutchisone,Yi-ChaoZouf,JinZouf,ColinL.Rastona*
a. InstituteforNanoscaleScienceandTechnology,CollegeofScienceandEngineering,FlindersUniversity,Adelaide,SA5042,Australia.
b. CentreforMarineBioproductsDevelopment,CollegeofMedicineandPublicHealth,FlindersUniversity,Adelaide,SA5042,Australia.
c. TraceAnalysisforchemical,EarthandEnvironmentalSciences(TrACEES),theuniversityofMelbourne,Victoria3010,Australia.
d. DepartmentofChemicalEngineering,CurtinUniversity,Perth,Australia.e. SchoolofPEMS,UniversityofNewSouthWales,ADFAcampus,CanberraBC,ACT2610,Australia.f. MaterialsEngineering,andCentre forMicroscopyandMicroanalysis,TheUniversityofQueensland,Brisbane,QLD
4072,Australia.
FigureS1.h-BN@magnetitecompositepreparedusingtheconfinedmodeofoperationoftheVFDfor15min,withpulsedlaseroperatingat1064nmand360mJ,irradiatingapureirontarget. Rotational speed at 7.5k rpm for a 20mmODglass tube, tilt angle 45º andh-BNdispersedinwater(0.1mg/mL).(a-f)SEMimagesand(g)XRDpattern.
Electronic Supplementary Material (ESI) for RSC Advances.This journal is © The Royal Society of Chemistry 2018
FigureS2.AFMimagesforh-BN@magnetitecompositepreparedinaVFDundercontinuousflowmodewithapulsedlaseroperatingat1064nmand360mJ,irradiatingapureirontarget.Rotationalspeedat7.5krpm,tiltangle45ºandflowrate1mL/min.
FigureS3.SEMimagesofh-BN@magnetitecompositepreparedundercontinuousflowmodewithapulsedlaserirradiatingapureirontarget,operatingat1064nmand360mJ,withthe20mmODglasstuberotatingat7.5krpm,tiltangle45oandflowrateat1mL/min.
FigureS4.BETchart(blue)ofh-BN@magnetitepreparedundercontinuousflowwithapulsedlaserirradiatingapureirontarget,operatingat1064nmand360mJ,withtheVFDtube20mm in diameter rotating at 7.5k rpm, tilt angle 45º and flow rate at 1mL/min; (red) asreceivedh-BN.
FigureS5. (a)EDXdataforelementalanalysis inbandc. (bandc)SEMimagesatvariouslocationsofh-BN@magnetitecompositepreparedundercontinuousflowwithapulsedlaserirradiatingapureirontargetoperatingat1064nmand360mJ,withaglasstube20mmindiameterrotatingat7.5krpm,tiltangle45ºandflowrateat1mL/min.
FigureS6.HRTEMimages(a-c)asreceivedh-BN,(d-f)h-BN@magnetitecompositepreparedusingapulsedlaserirradiatingapureirontargetoperatingat1064nmand360mJ,witha20mmglasstuberotatingat7.5krpm,tiltangle45ºandflowrateat1mL/min.
FigureS7.ATRFTIRspectraforasreceivedh-BNandh-BN@magnetitecompositecomparedwithmagnetitepreparedwithapulsedlaserirradiatingapureirontarget,operatingat1064nmand360mJwitha20mmODtuberotatingat7.5krpm,tiltangle45ºandaflowrateofwaterat0.1mL/min.1Theh-BN@magnetitewaspreparedasforthemagnetitebutwithh-BNdispersedinwater(0.1mg/mL)ataflowrateof1mL/min.
Controlexperiments:Threecontrolexperimentswereundertakentodecoupleanyeffectof
the laser on the h-BN and shear stress in the dynamic thin film in the VFD, with the
characterizationofthematerialusingSEMandXRD,andzetapotential.
1- Processingh-BNintheVFDintheabsenceofapulsedlaser.h-BNdispersedinwater(0.1
mg/mL)wasdeliveredviaajetfeedtothebaseofaglasstube20mmindiameterusing
ajetfeed,withtheflowrateat1mL/min,rotationalspeed7.5krpmandtiltangle45o.
Thecoloroftheprocessedliquidwassimilartothepre-processedsample,withthezeta
potentialsimilarat-19.7mV.
FigureS8.(a,b)SEMimagesforh-BNprocessedintheVFDundercontinuousflowwithaflowrateofadispersionofh-BNinwater(0.1mg/mL)at1mL/min,rotationspeed7.5krpm, tilt angle45o in theabsenceofa laser. (c)Photographof thedispersionofh-BNsolutionafterprocessing.(d)XRDoftheh-BNafterprocessing.
2- Processingwith thepulsed laser irradiating the solutionwithout irradiating the iron
target.Adispersionofasreceivedh-BNinwater(0.1mg/mL)wasdeliveredtothebaseof
a20mmODglasstubeat1mL/min,withthetuberotatingat7.5krpmandatatiltangle
of45o;thepulsedlaserwasoperatedat1064nmand360mJ.Thecoloroftheprocessed
liquidwassimilar to thepre-processedsample,witha similar zetapotentialvalueat -
18.4mV.
FigureS9.(a,b)SEMimagesforh-BNprocessedinaVFD,withadispersionoftheasreceivedmaterialdeliveredtothebaseofa20mmODglasstuberotatingat7.5krpm,ataflowrateofadispersionofh-BNinwater(0.1mg/mL)at1mL/minforatiltangleof45ºandthepulsedlaser operating at 1064 nm and 360 mJ, without the laser irradiating the iron rod. (c)Photographoftheprocesseddispersionofh-BN.(d)XRDofh-BNafterprocessing.
3- Confinedmodeprocessingofamixtureofh-BNwithIONPs(magnetitenanoparticles).
Amixtureofh-BNdispersedinwater(0.1mg/mL)andpreformedmagnetiteparticles(0.5
mg/mL)previouslyprepared in theVFDusingour recently reportedprocedure for the
exclusiveformationofthismaterial.1Thetotalvolumeofliquidinthetubewas1mL,with
therotationalspeedsetat7.5krpm,thetiltangleat45o,andtheprocessingtimeat15
mins,intheabsenceofalaser.Thecoloroftheresultingsolutionwasbrown,asexpected,
andtheSEMimagessimilartoh-BN@magnetitecompositeprepared insitu.However,
the zeta potential had two peaks, -8.03 mV and -17.3mV, presumably the former
corresponding with some of the h-BN particles devoid of surface bound magnetite
particles,notingthatthelatterisclosetozetapotentialforasreceivedh-BN(-19.7mV).
Incontrastthezetapotentialforh-BN@magnetiteprepareddirectlyinthepresenceofa
laseris+or-?37.2mV.
FigureS10.(a,b)SEMimagesforthematerialformedonprocessing1mLofamixtureofh-BN dispersed in water (0.1 mg/mL) and magnetite nanoparticles (0.5 mg/mL), using theconfinedmodeofoperationoftheVFD(15mins,45otiltangle,7.5krpmrotationalspeed,20mmODglasstube),intheabsenceoflaserirradiation.Themagnetitenanoparticles(12nmindiameter)wherepreparedusingourpublishedprocedureintheVFD.1(c)Photographoftheh-BN@magnetitesolutionafterprocessingundertheseconditions.
FigureS11.IndividualamountofPO43-adsorbedinmgL-1byeachsequentialcycle,forthreedifferentloadingsofmagnetich-BNsamples:(1)10mgadsorbent(light-greycolumns);(2)25mgadsorbent(dark-greycolumns);and(3)50mgadsorbent(blackcolumns).
1. X.Luo,A.H.M.Al-Antaki,T.M.D.Alharbi,W.D.Hutchison,Y.-c.Zou,J.Zou,A.Sheehan,W.ZhangandC.L.Raston,
ACSOmega,2018,3,11172-11178.