Scanning Nonlinear Dielectric Microscopy Woodhead Publishing Series in Electronic and Optical Materials Scanning Nonlinear Dielectric Microscopy Investigation of Ferroelectric, Dielectric, and Semiconductor Materials and Devices YASUO CHO WoodheadPublishingisanimprintofElsevier TheOfficers’MessBusinessCentre,RoystonRoad,Duxford,CB224QH,UnitedKingdom 50HampshireStreet,5thFloor,Cambridge,MA02139,UnitedStates TheBoulevard,LangfordLane,Kidlington,OX51GB,UnitedKingdom Copyright©2020ElsevierLtd.Allrightsreserved. Nopartofthispublicationmaybereproducedortransmittedinanyformorbyanymeans, electronicormechanical,includingphotocopying,recording,oranyinformationstorageand retrievalsystem,withoutpermissioninwritingfromthepublisher.Detailsonhowtoseek permission,furtherinformationaboutthePublisher’spermissionspoliciesandour arrangementswithorganizationssuchastheCopyrightClearanceCenterandtheCopyright LicensingAgency,canbefoundatourwebsite:www.elsevier.com/permissions. Thisbookandtheindividualcontributionscontainedinitareprotectedundercopyrightby thePublisher(otherthanasmaybenotedherein). Notices Knowledgeandbestpracticeinthisfieldareconstantlychanging.Asnewresearchand experiencebroadenourunderstanding,changesinresearchmethods,professionalpractices, ormedicaltreatmentmaybecomenecessary. Practitionersandresearchersmustalwaysrelyontheirownexperienceandknowledgein evaluatingandusinganyinformation,methods,compounds,orexperimentsdescribed herein.Inusingsuchinformationormethodstheyshouldbemindfuloftheirownsafety andthesafetyofothers,includingpartiesforwhomtheyhaveaprofessionalresponsibility. Tothefullestextentofthelaw,neitherthePublishernortheauthors,contributors,or editors,assumeanyliabilityforanyinjuryand/ordamagetopersonsorpropertyasamatter ofproductsliability,negligenceorotherwise,orfromanyuseoroperationofanymethods, products,instructions,orideascontainedinthematerialherein. BritishLibraryCataloguing-in-PublicationData AcataloguerecordforthisbookisavailablefromtheBritishLibrary LibraryofCongressCataloging-in-PublicationData AcatalogrecordforthisbookisavailablefromtheLibraryofCongress ISBN:978-0-12-817246-9(print) ISBN:978-0-08-102803-2(online) ForinformationonallWoodheadPublishingpublications visitourwebsiteathttps://www.elsevier.com/books-and-journals Publisher:MatthewDeans AcquisitionsEditor:KaylaDosSantos EditorialProjectManager:EmmaHayes ProductionProjectManager:AnithaSivaraj CoverDesigner:MatthewLimbert TypesetbyMPSLimited,Chennai,India Contents Preface ix 1. Principlesof scanning nonlinear dielectric microscopy for measuring ferroelectric anddielectric materials 1 1.1 Basictheory 1 1.2 Systemsetupofscanningnonlineardielectricmicroscopy 6 1.3 Theoryfornonlineardielectricimaging 9 1.4 Higher-orderscanningnonlineardielectricmicroscopy 16 References 21 2. Ferroelectric polarization measurement 23 2.1 Analysisofdistributionsofferroelectricdomainsonamicroscopicscale usingscanningnonlineardielectricmicroscopy 23 2.2 Higher-ordernonlineardielectricanalyses 26 References 37 3. Three-dimensionalpolarization measurement 39 3.1 Basicsofthree-dimensionalpolarizationdistributionassessment 39 3.2 Principlesofthree-dimensionalpolarizationassessmentusingscanning nonlineardielectricmicroscopy 39 3.3 LateralassessmentbyKelvinforcemicroscopywithelectricfieldcorrection 42 3.4 Lateralnanoscaleassessmentwithelectricfieldcorrection 46 References 48 4. Ultrahigh-density ferroelectric data storage using scanning nonlinear dielectric microscopy 49 4.1 Ferroelectricprobememorybasedonscanningnonlineardielectric microscopywithalinearscanningstage 49 4.2 Hard-disk-drive-typescanningnonlineardielectricmicroscopyferroelectric probememory 59 References 70 v vi Contents 5. Linear permittivitymeasurement by scanning nonlinear dielectric microscopy 75 5.1 Basicsoflinearpermittivityimagingusingcantilever-andneedle-type scanningnonlineardielectricmicroscopy 75 5.2 Quantitativelinearpermittivityimagingwithneedle-typescanning nonlineardielectricmicroscopy 77 5.3 Quantitativelinearpermittivitydeterminationusingcantilever-type scanningnonlineardielectricmicroscopy 80 References 91 6. Noncontact scanning nonlinear dielectric microscopy 95 6.1 Basicsofnoncontactscanningnonlineardielectricmicroscopy 95 6.2 Assessmentsofatomicdipolemomentsusingnoncontactscanning nonlineardielectricmicroscopy 99 References 111 7. Scanning nonlinear dielectric potentiometry for measurement of the potential induced byatomicdipolemoments 113 7.1 Principlesofscanningnonlineardielectricpotentiometry 113 7.2 Determiningatomicdipolemomentsatinterfacesbetweengraphene andSiCsubstratesbyscanningnonlineardielectricpotentiometry 124 References 137 8. Principles of scanningnonlinear dielectric microscopy for semiconductormeasurement 141 8.1 Thebasisforsemiconductoranalysisbyscanningnonlineardielectric microscopy 141 8.2 Basicaspectsofsemiconductoranalysisbyscanningnonlineardielectric microscopy 142 8.3 High-sensitivityscanningnonlineardielectricmicroscopyfordopant profiling 144 8.4 Avoidingthecontrastreversalissue 148 References 151 9. Carrier distribution measurement insemiconductor materials and devices 153 9.1 Assessmentsofthedistributionsofcarriersinmonocrystallineand amorphoussiliconsolarcells 153 9.2 AssessmentsofpolarizationandcarriersinGaNHEMTs 162 Contents vii 9.3 Contrastgenerationduringscanningnonlineardielectricmicroscopy imagingoffixedchargesatametaloxide(cid:1)nitrideoxidesemiconductor interface 167 References 171 10. Super-higher-order scanning nonlinear dielectric microscopy 175 10.1 Basicsofsuper-higher-orderscanningnonlineardielectricmicroscopy 175 10.2 ExaminingthedepletionlayerinaMOSFET 176 10.3 Analysisofcarriertypesandthedepletionlayerinamorphousand monocrystallineSisolarcellsbysuper-higher-orderscanningnonlinear dielectricmicroscopy 181 10.4 Usingsuper-higher-orderscanningnonlineardielectricmicroscopyto assesscarrierredistributioninoperationalSiCpowerdouble-implanted MOSFETsbasedongate-sourcevoltage 183 References 187 11. Local deep-level transient spectroscopy 189 11.1 Localdeep-leveltransientspectroscopy 189 11.2 Applyinglocaldeep-leveltransientspectroscopytotrapassessment 199 References 217 12. Time-resolved scanning nonlineardielectric microscopy 221 12.1 Thebasicsoftime-resolvedscanningnonlineardielectricmicroscopy 221 12.2 High-resolutionanalysisofSiO /4H-SiCinterfacesubsurfacedefectsusing 2 localdeep-leveltransientspectroscopybasedontime-resolvedscanning nonlineardielectricmicroscopy 232 References 237 Index 239 Preface Scanning nonlinear dielectric microscopy (SNDM) was invented in 1994 in Yamaguchi, Japan. Originally it was developed for investigating ferro- electric and dielectric materials with rather small nonlinear dielectric effects through the detection of capacitance variations caused by an applied voltage, that is, dC/dV. Thus since its early days, SNDM has featuredpaffiffiffihffiffiffiigh sensitivity to capacitance variation, on the order of 10222F= Hz. SNDM can easily measure nanoscale ferroelectric domains under ambient conditions and even atomic-scale dipole moments under ultra- high vacuum conditions. Moreover, as an application of SNDM to next- generation ultrahigh-density memory devices beyond the magnetic hard disk drive (HDD) and semiconductor flash memory, an investigation of ultrahigh-density ferroelectric data storage based on SNDM has been extensively investigated. As SNDM has a high sensitivity to capacitance variation, it is also very effective at characterizing semiconductor materials and devices. It can eas- ily distinguish the dopant type (PN) and has a wide dynamic range of sen- sitivity to both low and high concentrations of dopants. It is also applicable to the analysis of compound semiconductors with much lower signal levels than Si. We can avoid errors due to the two-valued function (contrast reversal) problem of dC/dV signals using dC/dz-SNDM. Extended versions of SNDM have been developed, such as superhigher- order SNDM, local-deep-level transient spectroscopy, noncontact SNDM, and scanning nonlinear dielectric potentiometry. The favorable features of SNDM originate from its significant sensitivity. Thus this book will meet the needs of those researchers in the indus- try, as well as academics and students, involved in the fields of ferroelec- trics, dielectrics, semiconductors, and scanning probe microscopy. This book will help those intending to investigate the ferroelectric nanodomain structure, which cannot be resolved by conventional piezo- response force microscopy (PFM), and the atomic dipole moment, which cannot be distinguished by conventional Kelvin probe force microscopy (KPFM), to realize ultrahigh-density ferroelectric data storage with much higher memory densities compared to flash memories and magnetic HDDs, to visualize the dopant distribution in the fine structure of ix x Preface state-of-the-art mutualized semiconductor devices, to visualize linear permittivities with higher resolution than other capacitance microscopies, to perform operand measurements of the carrier distribution of working semiconductor devices, to visualize the depletion layer distribution of semiconductor devices that cannot be measured by other methods, to visualize the two-dimensional trap (interface state of density, D ) distribu- it tion at the MOS interface, which has never been visualized by other techniques, and to measure real-time (ns range) carrier movement in semiconductor materials and devices. This book about SNDM gives new insight into the material and device physics of ferroelectrics, dielectrics, and semiconductors, which has proven hard to obtain by other methods. The author would like to acknowledge the many colleagues and stu- dents who have collaborated with and assisted the author in developing many advanced types of SNDM. Finally, the author wishes to thank his family for their kind encourage- ment. Without their support and understanding, this book would not be have been published. Yasuo Cho Research Institute of Electrical Communication, Tohoku University September 2019 CHAPTER 1 Principles of scanning nonlinear dielectric microscopy for measuring ferroelectric and dielectric materials 1.1 Basic theory 1.1.1 Macroscopic phenomenological definition of linear and nonlinear dielectric constants The relationship between the electric field and electric displacement in a nonlinear dielectric material with a fixed spontaneous polarization Ps is defined as follows. When we focus on the dielectric effects and disregard the effects associated with piezoelectricity and elasticity, the differential relationship for the internal energy function in the dielectric material can be expressed as [1(cid:1)3] dU5EidDi1θdσ; (1.1) where Ei and Di denote the ith (i51, 2, 3) component of the electric field and the electric displacement, respectively, and θ and σ are the tem- perature and entropy, respectively. In the above and below equations, we employed the Einstein convention that a repeated suffix represents a sum- mation with respect to that suffix. As the internal energy is determined/governed by the independent variables Di and σ, it is somewhat inconvenient for deriving the defini- tions of the dielectric constants. To change the independent variable from Di to Ei, we define the electric enthalpy H2 as [1,2] H2 (cid:3) U2EiDi (1.2) with its differential form given by dH252DidEi1θdσ: (1.3) ScanningNonlinearDielectricMicroscopy ©2020ElsevierLtd. DOI:https://doi.org/10.1016/B978-0-12-817246-9.00001-7 Allrightsreserved. 1