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Indian Institute of Metals Series Gunturi Venkata Sitarama Sastry Microstructural Characterisation Techniques Metallurgy Materials Engineering Indian Institute of Metals Series EditorialBoard DivakarRamachandran,IndiraGandhiCentreforAtomicResearch,Kalpakkam, India BikramjitBasu,IndianInstituteofScience,Bengaluru,India IChattoraj,NationalMetallurgicalLaboratory,Jamshedpur,India N.EswaraPrasad,DMSRDE,PODMSRDE,MinistryofDefence,GovtofIndia, Kanpur,UttarPradesh,India IndranilManna,IndianInstituteofTechnology,Kharagpur,India AmolA.Gokhale,IndianInstituteofTechnologyBombay,Mumbai,India G.MadhusudanReddy,DefenceMetallurgicalResearchLab,Hyderabad, Telangana,India AbouttheBookSeries: The study of metallurgy and materials science is vital for developing advanced materials for diverse applications. In the last decade, the progress in this field has beenrapidandextensive,givingusanewarrayofmaterials,withawiderangeof applications, and a variety of possibilities for processing and characterizing the materials. In order to make this growing volume of knowledge available, an initiativetopublishaseriesofbooksinMetallurgyandMaterialsSciencewastaken duringtheDiamondJubileeyearoftheIndianInstituteofMetals(IIM)intheyear 2006.TenyearslatertheseriesisnowpublishedinpartnershipwithSpringer. This book series publishes different categories of publications: textbooks to satisfy the requirements of students and beginners in the field, monographs on select topics by experts in the field, professional books to cater to the needs of practicingengineers,andproceedingsofselectinternationalconferencesorganized by IIM after mandatory peer review. The series publishes across all areas of materials sciences and metallurgy. An eminent panel of international and national experts acts as the advisory body in overseeing the selection of topics, important areastobecovered,andtheselectionofcontributingauthors. Gunturi Venkata Sitarama Sastry Microstructural Characterisation Techniques GunturiVenkataSitaramaSastry Formerly,Professor DepartmentofMetallurgicalEngineering andDeanofAcademicAffairs IndianInstituteofTechnologyBHU Varanasi,India ISSN 2509-6400 ISSN 2509-6419 (electronic) IndianInstituteofMetalsSeries ISBN 978-981-19-3508-4 ISBN 978-981-19-3509-1 (eBook) https://doi.org/10.1007/978-981-19-3509-1 ©TheEditor(s)(ifapplicable)andTheAuthor(s),underexclusivelicensetoSpringerNature SingaporePteLtd.2022 Thisworkissubjecttocopyright.AllrightsaresolelyandexclusivelylicensedbythePublisher,whether thewholeorpartofthematerialisconcerned,specificallytherightsoftranslation,reprinting,reuse ofillustrations,recitation,broadcasting,reproductiononmicrofilmsorinanyotherphysicalway,and transmissionorinformationstorageandretrieval,electronicadaptation,computersoftware,orbysimilar ordissimilarmethodologynowknownorhereafterdeveloped. Theuseofgeneraldescriptivenames,registerednames,trademarks,servicemarks,etc.inthispublication doesnotimply,evenintheabsenceofaspecificstatement,thatsuchnamesareexemptfromtherelevant protectivelawsandregulationsandthereforefreeforgeneraluse. Thepublisher,theauthors,andtheeditorsaresafetoassumethattheadviceandinformationinthisbook arebelievedtobetrueandaccurateatthedateofpublication.Neitherthepublishernortheauthorsor theeditorsgiveawarranty,expressedorimplied,withrespecttothematerialcontainedhereinorforany errorsoromissionsthatmayhavebeenmade.Thepublisherremainsneutralwithregardtojurisdictional claimsinpublishedmapsandinstitutionalaffiliations. ThisSpringerimprintispublishedbytheregisteredcompanySpringerNatureSingaporePteLtd. The registered company address is: 152 Beach Road, #21-01/04 Gateway East, Singapore 189721, Singapore Series Editor’s Preface TheIndianInstituteofMetalsSeriesisaninstitutionalpartnershipseriesfocusing onmetallurgyandmaterialsscienceandengineering. AbouttheIndianInstituteofMetals The Indian Institute of Metals (IIM) is a premier professional body (since 1947) representinganeminentanddynamicgroupofmetallurgistsandmaterialsscientists and engineers from R&D institutions, academia, and industry, mostly from India. Itisaregisteredprofessionalinstitutewiththeprimaryobjectiveofpromotingand advancingthestudyandpracticeofthescienceandtechnologyofmetals,alloys,and novel materials. The institute is actively engaged in promoting academia–research andinstitute–industryinteractions. GenesisandHistoryoftheSeries Thestudyofmetallurgyandmaterialsscienceandengineeringisvitalfordeveloping advancedmaterialsfordiverseapplications.Inthelastdecade,theprogressinthis fieldhasbeenrapidandextensive,givingusanewarrayofmaterials,withawide rangeofapplicationsandavarietyofpossibilitiesforprocessingandcharacterizing the materials. In order to make this growing volume of knowledge available, an initiativetopublishaseriesofbooksinmetallurgyandmaterialsscienceandengi- neeringwastakenduringtheDiamondJubileeyearoftheIndianInstituteofMetals (IIM)intheyear2006.IIMenteredintoapartnershipwithUniversitiesPress,Hyder- abad, and, as part of the IIMbook series,11 books were published, and a number ofthesehavebeenco-publishedbyCRCPress,USA.Thebookswereauthoredby eminentprofessionalsinacademia,industry,andR&Dwithoutstandingbackground intheirrespectivedomains,thusgeneratinguniqueresourcesofvalidatedexpertise v vi SeriesEditor’sPreface ofinterestinmetallurgy.Theinternationalcharacteroftheauthorsandeditorshas enabled the books to command national and global readership. This book series includesdifferentcategoriesofpublications:textbookstosatisfytherequirementsof undergraduatesandbeginnersinthefield,monographsonselectedtopicsbyexperts inthefield,andproceedingsofselectedinternationalconferencesorganizedbyIIM, aftermandatorypeerreview.Aneminentpanelofinternationalandnationalexperts constitutestheadvisorybodyinoverseeingtheselectionoftopics,importantareas tobecovered,inthebooksandtheselectionofcontributingauthors. CurrentSeriesInformation Toincreasethereadershipandtoensurewidedisseminationamongglobalreaders, this new chapter of the series has been initiated with Springer in the year 2016. Thegoalistocontinuepublishinghigh-valuecontentonmetallurgyandmaterials science and engineering, focusing on current trends and applications. So far, five important books on state of the art in metallurgy and materials science and engineering have been published and, during this year, two more books are released duringIIM-ATM2022.ReaderswhoareinterestedinwritingbooksfortheSeries maycontacttheSeriesEditor-in-Chief,Dr.U.Kamachi Mudali,Former President of IIM and Vice Chancellor of VIT Bhopal University at [email protected], [email protected] or the Springer Editorial Director, Ms. Swati Meherishi at [email protected]. Dr.U.KamachiMudali Editor-in-Chief SeriesinMetallurgyandMaterials Engineering Foreword Materialscharacterisationplaysacentralroleintheprocessinganddevelopmentof materialsingeneral,andmorespecificallyindevelopingadvancedmaterials.Thus,it becomesnecessarytoexposestudentstothesedifferenttechniquesatanearlystage oftheircareer.Nowonder,thisisarequiredcourseinmost(ifnotall)metallurgy andmaterialsscienceprogrammesbothattheundergraduateandgraduatelevels. Materialscharacterisationinvolvescharacterisingthematerialforitscrystalstruc- ture, microstructure and properties. Crystal structure determination is generally coveredinacourseonX-raydiffraction(althoughelectronmicroscopytechniques can also be used), while studying the properties of materials is done in more than onecourse,themechanicalpropertiesformanimportantcomponentofsuchasuite. Microstructural characterisation is perhaps the most critical and important of all these,thesubjectmatterofthepresentbookbyProfessorG.V.S.Sastry. Microstructuralcharacterisationistypicallydoneusingmicroscopytechniques— optical,scanningelectronandtransmissionelectronmicroscopyorotheradvanced microscopy techniques to unravel the structural features of materials at different levelsofresolution.Onecanobservethemicrostructuraldetailsattheverygrosslevel usingamagnifyingglass,oronafinerscaleusinganopticalmicroscope,andatstill finerlevelsusingascanningelectronortransmissionelectronmicroscope,oratan atomicscaleusingafieldionmicroscope.Theundergraduatestudentsarenotalways exposed to all the advanced techniques, even though they are expected at least to understandtheirbasicprinciples.Thestudentsshould,however,befullyfamiliarwith allthebasicmicrostructuralcharacterisationtechniques.ProfessorSastryprovides anoutstandingaccountoftheprinciples,operationandusageofthedifferenttypes of microscopes offering examples of the type of information that can be obtained alongwithwaysofinterpretingthemicrographsanddiffractionpatterns. Thereappeartobeafewspecialfeaturesofthisbook.OneisachapteronFourier Analysis and Fourier Transformations, which is typically not found in undergrad- uate textbooks (and not even in graduate textbooks). Further, optical microscopy is normally covered first and the concepts of electron microscopes are introduced to overcome the limitations of resolution limit available in an optical microscope. Another special feature of the book appears to be that Professor Sastry decided to vii viii Foreword providemostofthemicrographsandexamplesbasedontheworkdoneinIndiaor bypersonsofIndianoriginfromoverseas. ProfessorG.V.S.Sastryisanaccomplishedteacherwithlongexperience.Hehas beenapracticingelectronmicroscopistfornearly40yearsandthepresenttextbook reflectstheexperienceoftheauthorwhileexplainingsomeoftheimportantconcepts ofmicroscopy. TheUniversityinVaranasihasbeenameccaformicroscopyforalmost50years. ThefirstsummerschoolonMetallographywasconductedtherein1971,followed byseveralothersonElectronMicroscopyandFieldIonMicroscopyduringsubse- quentyears.Therefore,itisnotsurprisingthatthefirstundergraduatetextbookon MicrostructuralCharacterizationTechniqueshascomeoutfromVaranasi. Iamconfidentthatthisbookwillbewarmlywelcomedbythestudentsandfaculty alike.Iwishthebookagreatsuccess. Orlando,FL,USA C.Suryanarayana July2021 Acknowledgements MysincerethanksareduetothoseundergraduatestudentsofIIT(BHU),Varanasi, formerlyIT-BHU,Varanasi,whoseprobingquestionsandquerieshelpedmeagreat dealinimprovingthedeliveryofmyLecturesforaCourseonMetallographicTech- niques.Iamthankfultoallthosepost-graduatestudentswhochoseMaterialsChar- acterisation Techniques, and the post-graduate students and doctoral students who optedforAdvancedX-rayandElectronMicroscopyfortheirunquenchablethirstfor deeperknowledgeabouttheinterferenceofelectronwavesandaboutwhathappens totheirchargewhentheydosoetc.Theywereintriguedbythefactthatelectrons donotrepeleachotherwhentheyarefocussedtoaspot.Suchin-depthdiscussions happenedtobeanindirectmotivationformetowritethisbook.Akeyroleisplayed byProf.C.Suryanarayana,mentorformydoctoralstudy,inalltheknowledgeand experience I gained in electron microscopy. He used to answer untiringly all my endlessqueriesaboutelectronmicroscopyandelectrondiffraction.Ourlongdiscus- sionshelpedmepickupthethreadsintheinitialyears.Ioweagreatdealtohimfor makingmewhatIaminthefieldofelectronmicroscopy. The textbooks available for students in the early eighties were the classics, ElectronMicroscopyofThinCrystalsbyHirschetal.(Electronmicroscopyofthin crystalsbyP.B.Hirsch,A.Howie,R.B.Nicholson,D.W.PashleyandM.J.Whelan, Butterworth,London,1965)andFundamentalsofTransmissionElectronMicroscopy byHeidenreich(FundamentalsofTransmissionElectronMicroscopy,R.D.Heiden- reich, Interscience Publishers Inc.; First Edition (January 1, 1964)). The rigor of treatment in these two books was beyond the comprehension of undergraduates, Ifelt.However,Icouldn’tsitdowntowritethepresentbookatthattimeobviously. Duringmydoctoralresearch,IwasfortunatetohaveinteractionwithProf.G.Van Tendeloo,ReijksUniversitaireCentrum,Antwerpen,Belgium,whowasonavisiting assignmenttoourdepartment.Heintroducedmetothetechniquesofhigh-resolution electron microscopy and structure imaging. I am indeed grateful to him for the same.Imustacknowledgethecompanionshipandcompetitionprovidedinmyinitial ix