Metallization of Molybdenum Diselenide under Nonhydrostatic Compression - Liu et al. - 2021 - Unknown

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pubs.acs.org/JPCCArticleMetallizationofMolybdenumDiselenideunderNonhydrostaticCompressionBaoLiu,*LinLin,YangGao,YanzhangMa,PengyuZhou,DandanHan,andChunxiaoGao*CiteThis:J.Phys.Chem.C2021,125,5412−5416ReadOnlineACCESSMetrics&MoreArticleRecommendationsABSTRACT:Itisknownthatmetallizationcangreatlyfacilitatechemicalreactionsanddramaticallychangeelectrictransportpropertiesofmaterials.Thesearchformaterialsdisplayingmetallizationatlowpressureisoneofthemosturgentchallenges.Inthispaper,pressure-inducedmetallizationofmolybdenumdiselenide(MoSe2)undernonhydrostaticcompressionhasbeenstudiedexperimentallyusingHalleffectandX-raydiffractionmeasurementscombinedwithdiamondanvilcelltechniques.InsituconductivityandHalleffectmeasurementsunderpressurerevealamonotonicdecreaseofresistivitymostlyrelatedtoasignificantincreaseofthecarrierdensitybyafactorof4.Above35.7GPa,thesampleacquiresametalliccharacterwithacharacteristicincreaseofthemobilityfrom9.9to16.2cm2V−1·s−1andsaturationofthecarrierconcentrationat5.1×1020cm−3.TheseresultsshowthatthemetallizationofpowderMoSecanbe2initiatedbyareducedpressureof35.7GPaundernonhydrostaticcompression,comparedtothatabove40GPawithasingle-crystalsampleunderhydrostaticcompression[Nat.Commun.2015,6,7312].Themechanismsofanisotropic-stress-inducedmetallizationforsuchreducedinitiationpressurehavebeendiscussed.1.INTRODUCTIONbeenperformedusingbothexperimentalandtheoretical9−11methods.Sugaietal.measuredtheinsituhigh-pressureTransition-metaldichalcogenides(TMD),MX2(M=Mo,W,Ti,Nb,Ta,etc.,X=S,Se,Te,etc.)havebeensubjectedtoRamanspectraofMoSe2andshowedthatnoclearindicationmanytheoreticalandexperimentalstudiesbecauseoftheirofstructuralphasetransitionofMoSe2wasdiscoveredupto1612DownloadedviaBUTLERUNIVonMay16,2021at10:13:17(UTC).continuouslytunableelectronicstructuresandbandgaps.TheGPa.Aksoyetal.carriedoutinsituhigh-pressureX-raystructuresofTMDsshareaquasi-laminarmodeloftwo-diffraction(XRD)measurementsofMoSe2andillustratedthat13dimensional(2D)sheetsstackedontopofoneanother.Eachnostructuralphasetransformationoccurredupto35.7GPa.sheetconsistsofthreelayers,atransition-metalatomlayerinDaveetal.examinedthevariationofelectricalresistanceofSeehttps://pubs.acs.org/sharingguidelinesforoptionsonhowtolegitimatelysharepublishedarticles.themiddleandtwochalcogenatomlayerscovalentlybondedsingle-crystalMoSe2withpressureanddiscoverednoabnormal114tothetransition-metalatomsasthetopandbottomlayers.behaviorupto6.5GPa.However,previoustheoreticalThesesheetsareheldtogetherbyweakvanderWaalsforcescalculationshavepredictedthattheelectronicpropertiesofandshowexcellentmechanicalpropertiessuchashighMoSe2canbealteredinacontrollablemannerbyapplying2lubrication.Thecombinationofthecovalentbondswithinhydrostaticpressureduringthemetallizationprocessfrom28layersandvanderWaalsinteractionsbetweensheetsresultsinto40GPawhilemaintainingthe2Hstructure.15Recently,chighlyanisotropicphysicalpropertiesinTMDs.SuchsuchpredictionhasbeenverifiedexperimentallybyZhaoetcharacteristicisofgreatsignificanceinvariousapplications,al.,16whoseworkshowsthatsinglecrystalsofMoSemetalize3,42suchashydrogenevolutionreactioncatalysis,2Dmonolayerwithoutanystructuraltransitionatpressuresabove40GPa56solarcells,andultrafastlithium-ionstoragebatteries.underhydrostaticcompression.SuchdiscoverysuggeststhatFurthermore,severalmethods,includingintercalation,layerconfinement,chemicalvapordeposition,andstress,havebeenprovedvalidinthecontinuousmodificationoftheelectricReceived:January12,2021propertiesofTMDsandaffectingtheperformanceofTMDRevised:February9,2021devices.7Thus,featureshavedramaticallyextendedthePublished:February25,2021potentialapplicationsofTMDmaterialsinvariousareas.8Asapromisingcandidateforsolarcells,vastinvestigationsinoptical,structural,andelectronicresponsesofMoSe2have©2021AmericanChemicalSocietyhttps://dx.doi.org/10.1021/acs.jpcc.1c002795412J.Phys.Chem.C2021,125,5412−5416

1TheJournalofPhysicalChemistryCpubs.acs.org/JPCCArticlecontinuouslytuningTMDmaterials’electronicstructurebyutilize,insteadofavoiding,thenaturethatadiamondanvilcellmeansofpressureisfeasibleandofgreatpotentialingeneratesnonhydrostaticstresstostudythemetallizationofoptoelectronicandphotovoltaicapplications.MoSe2.OurgeometryofthesamplechamberandthenatureofMeanwhile,diversebehaviorsunderdifferentstresscon-uniaxialstresscanmakethesample’sregionreachaquasi-ditionsarecommonlyobservedinlaminarorquasi-laminarhomogeneouspressuredistributionforperformingreliableX-171819−21materials,suchas2Dgraphene,WS2,andMoS2.TheraydiffractionandHalleffectmeasurements.WS2powderundergoesisostructural2Hcto2Hametallizationundernonhydrostaticconditions,whichisnotobservedunder3.RESULTSANDDISCUSSION18hydrostaticconditions.ThetotalenergycalculationFigure1showstheisobarictemperaturedependenceofpredictedthatmonolayer2H-MoS2remainsstabletill67.9electricalresistivityinthetemperaturerangeof80−290K.19GPa,whereasinsitupressureandtemperature-dependentelectricalresistivitymeasurementsbyNayaketal.indicatedthatmultilayerMoS2undergoesanelectronictransitionfromasemiconductivetoametallicstateat19GPaunderhydrostatic20compresison.Yet,asreflectedinanotherinsitupressure-dependentresistivitymeasurementswithnopressure-trans-mittingmedium,MoS2powdersamplesfirstunderwentanisostructuralphasetransitionfroma2Hcto2Hastructure,after21whichtheybecamemetallicat28GPa.ThesestudiesallsuggestthatthebehaviorsofTMDmaterialsdependonboththestateofstressandthemorphologyofthesample.DespitetheintriguingdiversityofTMDmaterials’responsetodifferentstressconditions,whethersuchregulationappliestoMoSe2andthemechanismsbehinditremainunclear.Inthispaper,theabovementionedissueswereaddressedbycombininginsituelectricaltransportmeasurementswithinsituFigure1.TemperaturedependenceoftheresistivityofMoSe2atsynchrotronXRDmeasurementsinpowderMoSe2underrepresentativepressures.nonhydrostaticcompression.TheresultsindicatethatthemetallizationofMoSe2canbeinitiatedatareducedpressureof35.7GPaundernonhydrostaticcompressioncomparedtothatThetemperature(T)−resistivity(ρ)curvesexhibitalinearunderhydrostaticcompression(>40GPa).TheinsituHallrelationship.Atlowerpressures(<35.7GPa),theelectricaleffectmeasurements,ontheotherhand,providedadeeperresistivityofMoSedemonstratestypicalsemiconductor2interpretationfortheanisotropic-stress-inducedmetallization.characteristics,showingaconstantdecreasingtrendwithincreasingtemperature.Thedecreasingratetendstobe2.EXPERIMENTALMETHODSreduced,evenapproachingzeroataround35.7GPa.AtThecommerciallyavailableMoSe2powder(AlfaCo.,purityofpressuresabove35.7GPa,apositivetemperaturedependence99.8%)wasloadedintoanonmagneticdiamondanvilcellwithisobserved,indicatingtheinitiationofmetallizationofMoSe2.theanvilculetof400μmdiameter.AsheetofrheniumusedasComparedwiththemetallizationofasingle-crystalMoSe2agasketwaspreindentedto40μmthickness.Aholewith200reportedabove40GPaunderhydrostaticcompressionusing16μmdiameterwasdrilledatthecenteroftheindentationbyancubicBNasapressure-transmittingmedium,suchresultelectricdischargemachineandservedasthesamplechamber.showsthattheinitiationpressureofmetallizationunderApieceofarubychipofaround5μmwasusedforpressurenonhydrostaticconditionsislowerthanthatunderhydrostaticcalibration.Afour-probeMofilmmicrocircuitwithavanderconditions.PauwconfigurationwasusedforinsituelectricaltransportTogaindeeperinsightintotheanisotropic-stress-inducedmeasurementsunderpressure.Theelectrodemanufacturing,metallizationandthecarriertransportationforMoSe2,electricalinsulation,magneticcalibration,andotherrelevantnonhydrostaticcompressionHalleffectmeasurementswereexperimentaldetailshavebeenreportedinourpreviousalsoconducted.AsshowninFigure2,atambientconditions,22−24studies.Thesamplethicknessunderpressurewastheelectricalresistivity,carrierconcentration,andmobilityaremeasuredbyamicrometerwiththeaccuracyof0.5μm,30.1Ω·cm,6.57×1015cm−3,and31.57cm2V−1s−1,duringwhichthedeformationoftheanvilswasincludedasarespectively.Themagnitudeofρandninourexperimentsis2514correction.comparablewithpreviousresults.AsshowninFigure2a,theInsituhigh-pressureXRDexperimentswerecarriedoutresistivityofMoSe2decreasesconsiderablybymorethan4usingasynchrotronX-raysource(λ=0.6199Å)atthe4W2ordersofmagnitudewhenthepressurewasincreasedfromHigh-PressureStationofBeijingSynchrotronRadiationambientto34.2GPa.TheresistivityofMoSe2thenchangesitsFacility(BSRF).Thediffractiondatawerecollectedusinganpressuredependenceat∼35.7GPaanddecreasesgraduallytoMAR165CCD.Theintensityversusdiffractionanglepatterns38.8GPa.Duringdecompression,followingahysteresiscycle,weregeneratedfromXRDimagesusingFIT2Dsoftware.Fortheabnormalchangereemergesat26.5GPa,andresistivitynonhydrostaticcompressionandbetterelectrodecontact,nodoesnotgetrestoredtoitsoriginalmagnitudeatambientpressure-transmittingmediumwasusedinbothXRDconditions.measurementsandHalleffectmeasurements.AlthoughAsshowninFigure2b,c,fromanambientconditionto34.2extensiveeffortshavebeendedicatedtogeneratingtheGPa,thecarrierconcentrationincreasesbymorethan5ordershydrostaticpressuresinadiamondanvilcellbychoosingofmagnitude,whilecarriermobilitydecreasessmoothly.Thevariouspressuremediums,thisexperimentalapproachistoincreasedcarrierconcentrationcanonlybepartlycompensated5413https://dx.doi.org/10.1021/acs.jpcc.1c00279J.Phys.Chem.C2021,125,5412−5416

2TheJournalofPhysicalChemistryCpubs.acs.org/JPCCArticleFigure2.Electricalresistivity(a),carrierconcentration(b),andmobility(c)ofMoSe2asafunctionofpressureatroomtemperature.bythedecreasedcarriermobility,whichistheprimarycauseofdramaticreductionofelectricalresistivitybelow34.2GPa.Uponfurthercompression,bothcarrierconcentrationandFigure3.(a)RepresentativeXRDpatternsatvariouspressureswithmobilityshowabnormalchangesat∼35.7GPa.Carriernopressuremediumand(b)pressuredependenceoftheunitcellmobilityinvertstopositivepressuredependencewhiletheparameter.Theerrorswithinthesymbolswerereceivedfromtherefinementofcellparameters.carrierconcentrationseemstoreachsaturation.Consequently,theelectricalresistivityofMoSe2decreasessmoothlyabove35.7GPa.Duringdecompression,bothcarrierconcentrationseverepressure-inducedlinebroadeningisobservedwithandmobilityofMoSe2changeabnormallyat26.5GPaanddoanisotropic-stresselevation.Suchbehaviorisascribedtotwonotgetrestoredtotheirinitialvalueswhenquenchedtosources,anisotropic-stress-inducedcomminutionandmicro-ambientconditionsduetothehysteresiseffect.strainofsamplecrystallites.SincetheintroductionofInordertounderstandthestructuralchangeinnon-anisotropicstressusuallyresultsinthecomminutionofthehydrostaticconditions,XRDmeasurementswerecarriedouttocrystallites,suchphenomenoneffectivelyreducesthecoherentmonitorthestructuralvariationofMoSe2.Figure3ashowsthescatteringdomainsizeofthesampleandcontributestolineselectedXRDpatternsofMoSe2withnopressure-transmittingbroadening.Furthermore,thelinebroadeningisalsoenhancedmedium.Atinitialpressureof1.4GPa,thepatternofMoSe2bytheappearanceofthemicrostrainsinthecrystallitesunder26canbewellindexedintothe2Hhexagonallayeredcrystalnonhydrostaticcompression.Duringdecompression,diffrac-structure(P63/mmc),asseeninthepreviouslyreportedresulttionpeaksaregraduallyrestoredtotheiroriginalposition,13underhydrostaticpressure.Itisdiscoveredthat,withwhilethebroadenedpeakwidthismaintained,indicatingthatincreasingpressure,thediffractionlinescontinuouslyshifttothecomminutionoftheMoSe2crystallitesafteranisotropic-larger2θvaluesduetocontractionofthelattice.Nonewpeakstresstreatmentsisnotrecovered.TheXRDresultswithnoisobservedinthepressurerangeoftheexperiment.Thepressuremediumshowthatnostructuraltransformationhadpressuredependenceofthelatticeparametersispresentedinoccurredinthispressurerange,whichalsocorrespondsto16Figure3b.Thecellparametersshowasmoothcontinuoussimilarobservationswithaneonpressuremedium.There-decreasewithincreasingpressureandalsoshownoevidencefore,itisclearthatanisostructuralmetallizationprocessinforaphasetransitionundernonhydrostaticcompression.ThepowderMoSe2occurredundernonhydrostaticpressure.a-axisdecreasedby6.9%andthec-axisdecreasedby11.1%atThemetallizationcausedbyisotropicstresswasfirst2736.4GPa,whichindicatesmoretypicallyanisotropicdiscoveredbyMottandhasbeenknownastheMottcompressionbehaviorundernonhydrostaticconditions.Thetransition.InMotttransition,pressuretriggersthewavecellparametersareinagreementwiththoseofref13.Notethatfunctionsofthevalenceelectronstooverlap,whichresultsinforMoSe2underhydrostaticandnonhydrostaticcompression,theclosingofthevalence-conductionbandgapandthusthec-axisismuchmorecompressiblethanthea-axis.Themetallization.Ingeneral,forthesemiconductor,theincreaseinwidthofdiffractionlinesatnonhydrostaticcompressionispressureleadstoaphenomenonnamedstress-inducedlargerthanthatobtainedathydrostaticcompression.Moreimpuritylevels,inwhichatomsdeviatefromtheirequilibrium5414https://dx.doi.org/10.1021/acs.jpcc.1c00279J.Phys.Chem.C2021,125,5412−5416

3TheJournalofPhysicalChemistryCpubs.acs.org/JPCCArticlepositionsandbringaboutadditionalenergylevelsinbandofstress-inducedionization.Undernonhydrostaticconditions,gaps.Athighpressure,theelectricconductionisdominatedbyanisotropicstresscanclosethebandgapmoreefficientlythancarriersfrombothoverthefullbandgapsandthestress-thatunderhydrostaticcompressionbecauseoftheanisotropic-28inducedimpuritylevelsinthebandgaps.Suchmodelofstress-drivendeformationsofBrillouinzoneboundaries.stress-inducedionizationofimpuritylevelsisusuallyutilizedtounderstandtheeffectofhydrostaticpressureontheelectrical■29AUTHORINFORMATIONpropertiesofasemiconductor.Ontheotherhand,highCorrespondingAuthorspressurealsomakesconductionandthevalencebandstoBaoLiu−CollegeofScience,NortheastElectricPowerbroadenandthebandgaptobecomenarrow(asindicatedbyUniversity,Jilin132012,China;orcid.org/0000-0001-Eg′showninFigure4).Thus,morecarrierscanbeactivated8203-7955;Phone:+86-(0)432-6480-6621;Email:liubao@neepu.edu.cnChunxiaoGao−StateKeyLaboratoryofSuperHardMaterials,JilinUniversity,Changchun130012,China;orcid.org/0000-0001-5329-2623;Phone:+86-(0)431-8516-8878-601;Email:cc060109@qq.comAuthorsLinLin−DepartmentofMechanicalEngineering,TexasTechUniversity,Lubbock,Texas79409,UnitedStatesYangGao−DepartmentofMechanicalEngineering,TexasTechUniversity,Lubbock,Texas79409,UnitedStates;CenterforHighPressureScienceandTechnologyAdvancedResearch,Shanghai201203,China;orcid.org/0000-Figure4.Sketchfortheshiftoftheenergylevelundervariouskinds0003-4530-8570ofstresses.YanzhangMa−DepartmentofMechanicalEngineering,TexasTechUniversity,Lubbock,Texas79409,UnitedStatesPengyuZhou−CollegeofScience,NortheastElectricPowerfromavalencebandtoaconductionband.Therefore,theUniversity,Jilin132012,ChinaincreaseofthecarrierconcentrationofMoSe2withincreasingDandanHan−CollegeofScience,NortheastElectricPowerpressureupto35.7GPaiscausedbybothbandgapnarrowingUniversity,Jilin132012,Chinaandstress-inducedimpuritylevelsinbandgaps.Above35.7Completecontactinformationisavailableat:GPa,thesaturatedcarrierconcentrationsuggeststhatthehttps://pubs.acs.org/10.1021/acs.jpcc.1c00279impuritylevelsarewhollyionizedandbandscompletelyoverlapathigherpressure.UnlikehydrostaticcompressionthatcompressesallthreeNotesprincipalaxesofacrystallattice,nonhydrostaticcompressionTheauthorsdeclarenocompetingfinancialinterest.tendstocompressfewerlatticeaxes.Therefore,nonhydrostaticcompressionresultsinthedeformationofBrillouinzone■ACKNOWLEDGMENTSboundariesandshiftofbandgapmid-pointE0.Asaresult,theTheauthorsthankscientistsatBeamline4W2ofBSRFforindirectbandgapshrinkstoEg*(Eg*40GPa).Hallhydrogenevolutionreaction.Angew.Chem.,Int.Ed.2014,53,7860−effectmeasurementsshowedthatthedramaticreductionof7863.electricalresistivitybelow34.2GPaiscausedbyanincreased(5)Tsai,M.;Su,S.;Chang,J.;Tsai,D.;Chen,C.;Wu,C.;Li,L.;carrierconcentrationandgradualdescentofelectricalChen,L.;He,J.MonolayerMoS2heterojunctionsolarcells.ACSresistivityofthemetallicphaseofMoSe2duetothesaturationNano2014,8,8317−8322.5415https://dx.doi.org/10.1021/acs.jpcc.1c00279J.Phys.Chem.C2021,125,5412−5416

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