Hitachi HighTech“Tre produ: deszristion given herein apples as of Apri, 2008. Note that there is 8 posebilty of sala ofthe product hehe dscortinued without prior notice, or of paral change Inthe spearance or specifotons of the rout forimprovement Dil cathe ae popared for ooh of Un imtruments dewrbed, 29 plese igure wih our sles roresertatve if you woud the to obtain the,Table of Contents Chapter 1. What is the SEM? 1.1 What can we do with @ SEM? 112 Principle and Structure of the SEM ssseeserees 1.3 Procedure for SEM Observation Chapter 2. Sampling 24 Toole Used 22 Sanpling 23 Metal Coating 24 ton Ming ee Chepter 3. Let's Observe the Folowing with a SEM! 8.1 Machined Products, Materials 32 Seniconductor Wafer, Liquid Crystal Display 83 Bidlogical Samples 34 Foodsture Chapter 4 What causes these images? (Chapter 5.SEM Instruments Available seve ‘Chapter 6. Q8A for persons wanting to know more about the SEM! 6.1 Concerning formation of the electron beam «eeeseeseee 82 Concering Evacuation 6.3 Generation, detection and usage of SEM signal « 84 Viewing conditions for acquiring good SEM images «. 6.5 Principle and applications of low vacuum SEM... abst 8.8 Generation/detection of x-rays and elemental analysis method .-.63 6.7 How to improve accuracy in xray analysis «se+seeseesee een 68 Principle and application of STEM BChapter 1. What is the SEM? 4.1 What can we do with a SEM? ‘The resolving power of the human eye is around 0.1 mm. To ‘obsewve objects smaller than this, an optical micrescope or electron microscope must be used ee Bohm ~a "am ~00nmIm15ym BUNTON —~2mm Tamm ‘nen 10m 100em rm 104m 10042 trim 10mm, 100mm Eleciron microscopes are available in a scanning electron version (SEM)" and ¢ transmission electron version (TEM)?. The SEM is used particularly for observing the fine structure of a specimen surface at high ‘magnification, while the TEM is used mainly for observing the inner structure of a specimen at high magnification. We wil introduce here the features of the SEM, "7 SEW. Searing Eason Meraszope 172 Tete Tanai Eacron Mrorcope Features of the SEM 4. All slid surfaces can be observed in a range fom low to high magnifications. 2. Focal depthis greater than that ofan optical microscope, allowing Us to ‘scquire a storeoecopic mage. 3. Combination with an x-ay analyzer permits compositional analysis ofa mmicroscopicarea.Now let's compare the images cbtained with an optical microssope and the SEM. used is a fib blocking ultra iployed in parasols for 3t rays. ‘Sam Observation with optical ‘microscope Fiver obseried with an optical microscope Although the OM provides coor informaiton, thas @ shallow depth of focus, and when focusing onthe cried patin the image a the lef the portion having a sighty arent height comes out a8 an unctear image 140 magnification ‘Observation with SEM ‘The cample was observed with an ‘SEM at the same magnification 3s ‘sed with the OM. Although the ‘SEM image is back & white acks Color information), thas a greater depth of focus and provides stereoscopic information % 110 magnification “When further enlarged! % 4,000 mag. % 15,000 mag. |When observing an SEM image vith the magnification increased to 4,000, inogane matter (white particles) that are used to block UV rays can be seen dispersed in the ‘ber. Note that SEM images include secondary electron and backscattered electron information (explained later), and the above are secondary electron images. By further increasing magnification to 15,000, can be Seen thatthe inorganic mater bocomas paricles of 100 to 500 nm in size, A cross-sectional observation can be made nextlo See how the inarganic partcles are dispersed in the fiber.‘Observation and Compositional Analysis of Fiber Cross-section Backscattered electron image (5,000 magnification) ‘The cross-sectional structure of the fiber was observed wth a backscattered election detector This permits conformaton of how the white particles are dspersed in the foe, Let's put this to (compositional) analysis. (xray spectrum of area (ID X-ray mapping tenclosed in rectangle above image of C and Ti Fst of al, let's cu the fer observed before and observe is cross-sectional structure via a backscattered elec detector. Since a BSE image permis Getecting acifference in average atomic rumber as a dfference in contrat, a location having aiferent compositonal elements can be clearty seen. The white listening particles ae inorgaric matter, and one can see how they ae disperses inthe ber. Also, when an electon beam is applied to the sample, characteristic "rays wll be produced as well. By attaching tothe electron microscope an Xray ‘analyzer that captures these xrays, it can be seen what elements exist and where they ae located. ‘By conducting x-ray analysis onthe part enclosed in the rectangle onthe BSE image, itis seen rom the spectrum tha itanium (Ti exists inthe sample. Now, by conducting xray mapping on carbon (C) and Tiin the same visual field as on the BSE image, t wil be clear thatthe fber contains organic matter (C main) ‘and thal paricies of T (actually TIO) which serve to block UV rays are dispersed init4.2 Principle and Structure of the SEM - Lot's loam the principlo and etructure of the SEM. What s the SEM? ‘The SEM is an instrument that scens a sample surface witha finely converged electron ‘beam in a vacuum, detects the information (signals) produced at that ime from the ‘sample, and presents an enlargedimage ofthe sample surface on the monitor seen, Incident electron beam Backscattered electrons Cee er (BSE image) Cathodic light (CL image) Secondary electrons. (SE image) ‘Semple current Q ——* 77, | Sianals produced from sample By iaciating the sample wth an electron beam ira vacuum, secondary electrons, backscattered electrons, characteristic x-rays and other signals are generated ae indicated inthe figure above, The SEM mainly utlzes secondary electron of backscattered electron signals to form an image. Secondary electrons are produced near the sample surface, andthe SE image obtained upon detecting these electrons reflects the fine topographical strcture ofthe sample. Backscattered electrons are those refiected Upon striking the toms composing te sample, and the numer of these electrons le dependent onthe compostion {average atomic number, crystal orietaton, etc) ofthe sample, A BSE image therefore reflects the compostonal distribution onthe sample surface. Besides, an ‘ray detector can be mounted tothe SEM for corducing elemental analysis. So the SEM is usable not only for observing the sample structure, itis also applicable {38 an xray analyze for determining what elements are included inthe sample and tewnat degreeConfiguration of SEM‘As shown in the figure atthe lf, the SEM consists manly of column, specimen ‘chamber display and operating Secon. The interior ofthe column is Keptin a high ‘Yacuurm, and the electron beam produced by the electron gun (prior to stking the ‘Sampl) ie converged into a fe beam via the electromagnetic lenses (condenser and ‘bjectve lenses) And by applying a scan signal tothe defection cos, the electron ‘beam is scanned along the sample surface. ‘The specimen chamber is equiped wih a ‘specimen stage having @ specimen goniometer, a secondary electron detecor for detecting signals produced from the sample, and depending onthe instrument, & backscattered electron detector andlor an xray detector. Connected below the ‘specimen chamber isa vacuum pump for Keeping the interior ofthe column and, ‘Speomen chamber in @ high vacuum’ ‘A mechani hat ems eloctons rom a metal and accelerates them na strong electic fa Thee are tes ypes of electron gun sccorang othe method of emision — eld ‘emission ype (FE) electron gun, Sztoty electron gun and ermal laten gut Fer ‘eats refer to Chapter 6. “an eecomagnot Tos (co used to converge the electron beam emit fom the ‘locren gun into ate beam, 3 Deflection e “Aimachanlam used a scan he eaten beam in X and Y directions and change the area (reagiteaton to be scanned. The SEM magiication, 25 ndcatd in the fue is ‘termined by the rate of wh of image spay area (i) to width of electron bear sean on ‘he samp (W) ‘4. Objective lens ‘Used converge te electron beam nto a ine beam an focus tonto the sample surtace ‘Thee ate tee types of ng, ens, ser iniens and outens, acorang te object of bseriton or reslison. Referto Chapter 6 for etal. 1. Secondary electron detoctor rien captures, convo oleic signal and amples he secondary eecrons posed rom the sample. Rete 'o Chapter forthe metiod of aetcton 8. Display ‘Ganvers the detected and amplified secondary electron signal o brighiness and proves ‘enlarged mage. 7. Vacuum pump "Evaovatee te column and specimen chamber ta igh vacuum level (10 to 104 Pa. Refer to Chap or detalson evacuation.4.3 Procedure for SEM Observation ie inrouce here the procedure for SEM observation using the &-3400 SEM as anexamp (1) Startup of instrument (1) Tam ON power the instrument (2) Login to PC and hen startup the SEM sonwae '2) Preparation of sample to be observed (9) Atach conductive tape to specimen sub and hen mount the sample on this. Sample (Reterto Chapt 2 for detains i. Sete peptone) Specenen stub (4) Set specimen sub on exclusive alder and aust eight wih "nelgh gauge (Roferto nstructon manual of appeable strurent) [2 Setsng of sample to meoroscope (6) Press AIR on front gana of column and introduce air itospecimen chamber. (@) Pullout spocmen sage gent and set specimen rider on cote of sage (7) Press EVAC on ron pane of column and evacuate specimen chamber. (@) Wen evacuaton of specimen chamber is ished, stat ebseration of sare. ealoeae er iapmertamibemap ite oer 720 ue men onemeril no eos il ee eee (51 Acauistion and saving of image (12) Chek lion te ett sae itl nage (3) Sots apr oc map and Son G) evac/air swroh rnentioned in stops (BAN) at loftChapter 2. Sampling Introduced here i the general method of sample preparation (sampling). 2.4 Tools Used oS & 2.2 Sampling (1) Baik same, tm, sce etejar pear emriaetes eee sear Seen ue renege eteiochpe ape eee (4) Biological sample (6) Foodstus, samples 2 Pea : ‘containing oil 2 (rom eH) enn (Tanne eo aur wore, = (chara gat te) Dg a oso (ota palo. mee ioe septa nae apesia'o ieee aie fpttcrieneone 02.3 Metal Coating (1) Purposes of coatng “ Tomake te sample surface conducive (prevention of charge-up) * Toineresse the production rate of secondary electrons (ncrease image information) + To prevent damage to sample (2) Fim ticknoss oF coatng Atnough a telnet of overl nanometers i standard forthe fim coating, # vanes wth {he magnfeaton vss for he cbseration A somewhat thinner coating issuable for hhgh-magniieaton observation. And for observation at ow magnfeaton, Sight ticker ‘coating wil prove a clear mage having a good SIN rato. (©) Kinds of metal targets [Goa Fer Evaporation fim suitable gereratuce SEM obseraten ‘AsPs_ | Gottpataum | "Sen | Coating parece | 4 Fim ctuntor quality having propa | Pitinan 1 | adoqusialy fine parle salad torte: | Fhe | 2 Secandenelecren seu Sacharge tis good pee Eo 13. Stale apanstexsaton “The particles ofthe coating tim become tn n the ode ndatedin the above table. Ona sample coated wih gol, he paricles canbe cbserved at a maghifeaton of 5,000 0 “50,000 and nghe Fer thi esson agoltpaladum costing ofen used wih 8 genera Use SEM. inthe case of @ SEM having igh resolution such asthe FE-SEM, ate coating ‘mwah wen te pein cannes be taan i nid There sina oe parla Sn ofthe coating tim ares with he coatng ator, e argot must be slid in accordance wth he purpose Ao, fr coatng a sampie having an uneven sufac, ks recommended © ‘appl the coating 3104 times whiting te sample diferent drecions as shown the ‘gure below re agreton spring device ‘ostng oes having uneven surface +4) (carbon) coating ‘Avacuum evaporator is usualy empoyed for carbon coating. Since the parties of the evaperation fn ae fre an ofl densty, tis ype of coating issuable or ‘lometal analy or Soseraton of BSE Mapes24 Ion Milling (1) Whats on mang? Ton Bea ming technique tha ties @ broad lon beam (BIB) of approximately 1 mm in diameter cischarged from te gun to sputter stor from the sample surface is Used for elminaing machining flaws fom th sample curface or mpreparing se Soatonal samples of mull fim ayers (2) Wratis BiB on mating? 2-1 Surface processing lat miling method) ‘The sample surface is uniformly eehed by iradatngthe fon beam at an angle wie rotating the sample Man applications: * Ciminaion of oxte fim or contamination from a wie aes of about § mm eamster on ‘sample surtsce + Elman of machining faws trom machined sample surface {Opeenation of erst grins or aver ford by he! mang radiation of B18 stan angle (Outer view a M300 on ming device 2.2 Cross-section processing ‘An even eros secton covering a wie area (about 1x 1 mm) ofa sample canbe prepared by placing» shielding pata on the sample and blocking pat fhe on bean radiates onto the sample, then etrng sound the edge of he shiking plate, Main apleavons * Euaiaionlohesnstin of compe crm aun ued in machining = sample *Obsenatonianaies af mated boundary * Cross sectonal oservation of sample (papori, ol) susceptbie to stress 116 vertical eration oS saat ~ ‘a Sample sing ‘Outer vew of E500 ion ming daviesChapter 3. Let’s Observe the Following with a SEM! 3-4 Machined Products, Materials (1) [ittetas, eiectronic materials] ge some ere L eo “Romerang ota: Pricgaahig (etacmmae Sonne ‘nsclting mater Trai, coss-teion sample seniae obenes © ample: Resin packing machine samplePolymeric materials] Tneuaing rateral Tigi, emuion amp psgenible Sen hea Rubber tenes ‘made wih heh negav votae(deosesionvtap) is poled oe sala the acon bam ‘Serato vat eorton gy = Second jt vee hm sare ae tha mode pe ceeaion ‘sample aracas ander danage chor sow trivago 500V ose oe Cat wah ~oggeni syn Se RSF toy ese asain me oy angen a ifr cbanton wn *EaGp (acon Sac Pate [Eto le Smet of sachov beam tarkacaterng Staton, ay by escing We stam (50) at yews net Se cel ata of arin ocr fea canbe Gets ar mpg3-4 Machined Products, Materiale (2) [Ponder rere parices, nano materais —] Sa ae aS 6 Sapes of guP- Senples of nano oer Fine metalic partes ‘cata Ss. eaters'E [Wie ERE Sie emery an ea Sos Bincsion Sta marpe by mean ttn Cony fe STEM Ae.8-2 Semiconductor Wafer, Liquid Crystal play [Semiconductor] ‘Surfae opservaton ‘Grose-eacton observation Refer o secon on Samping or meted i popatg ee soon Wing sacs Wing structure (Eraeture cross seston) (te processes (posh secon)Liquid crystal wositee | | Sitinibaey ane ae awd on cee ‘oust Cage cos) pee | (Ee eo F== ¥ finer ons 08] (Pecorsgeleti 20) "st nece BEE nose (haart st ane (Rescctavetine 2 | itiereronen ass Sheewag oe rarciid {Geeta ns cots ‘Sheng conposter owe Spee ase messTriderwaterBoTogial matior a=) t= Coen) a Pees] |aenare bs ote xan Sagres Ae fu 98 teWicroorganieme angi) £ Retr to preceding page 10 for bicogical sample petreatmet method, = elec Searmeptcsiae3-4, Foodstuffs Food consti, processed tod suscep heat ‘Spinach Dc Fh napa 0 {oe oun eratin ‘Sage temperate 20° een e ares Conepetosame aChapter 4. What causes these images? ™ Image moves 660 © Sample structure cannot be discerned 600 Image is distorted & Image fluctuates 06 Brightness is unstable ©0006 ™ Cannot be focused ©6006 Effect of external disturbance@ ret is the charge-uo phenomenon? ‘Charge-up occurs dng cbsenaton of non-conducive sales. and may be conspicunus ‘especialy when scan speed of maghicaon schangod. Below are examples ofthe ‘Sharyerup phenonenn [Examples of Gnarge-up Phenomenon Cent etge te Inthe tectron beam inasaton area on te sample surface, tere ae an incoming etecron {ow ip and an outgoing eon Peo (10 ge * pe ha) neat inte 2D0¥6 ‘figures. When the sample surfaces conducive, 1's eq! op. Butwhen Be charge becomes unbalanced, Ip oes no =aualo, charge-p wil appear and the suace poten wary Folowing are countermeasures fot the charge-up phenomenon “Reduce he acclerstingvalace 2. Reduce te sample radiating current 23. Aeply a metal coating. 4 Integrate the image (rm an nage by superimposing images obtained at rapid scan) ‘5. Goserve mages now vacuum move 8. Utize a low-scsleraton BSE signal (lminate SE signal by means of signal varying mechanism). Refer 5 trough 4-10in Chaptr6 for detals.Qwratis contamination? ‘The phenomenon by whch gas molecubs of hydrocarbons existing around the sampe calect onthe sample de o electron beam iradiaton, then bond together and achere to ‘he sample sre i ered o a2 ‘contanaton (ee gure at the night), Wit tbe ‘secon beam iresang the same, the clanty ‘he mage at at area decreases s shown inthe igure below le and becomes dtr. “The reason forte datfness fought be “at the mater accumltd onthe sate “surface suppreseos the cecharge of seconsary ‘lectons fom the same Exar of Sample Cntairion “Te flowing sts ae required in order to reduce the contamination: "Reduction of residual gas moleules n specimen amber (mprovement of vacuum evel) + Redicton af gas molecules derives tm sample Cones meas io aver the above recns ea fos. 1: Use a minimum amount of conducive paste or ape when mounting the sample nthe instement “Thoroughly ery te conducbve past wha dyer orth ike proto Inserting sample into the nerument or obeonaton. 3. Heal ard dogas the sample na vacuum seve. 44 Camry out ecung as qk a8 possible and avo cbserving he sare locaton fr aong time especialy thigh maghiieabon 5. Observe samples whe cooing he sampe suroundings wih 2cald tap. “The reason why contamiatons conspicuous nthe eft sie ofthe electron beam scaning area's that time is proved in electron bea: cena fr the electrons tremain there. TO Preven a say magnets fl tom affecting th mago, a method of canning thats Synchronous wah the power frequency (50 or 0 Hz) 1 zed (power suppl synctronous san), ‘et reques a wating me bear the stato scan. A recent method of prevening is ‘Sonfamination eto equ the SEM wih a Beam danxng uncon wih wich the econ bear ‘Comet scl e sample reg tne wating tne bear the sant of sean a© What is beam damage? “Thomal change or chomical-hange occuring ona sample due to electron beam ination ‘atered teas beam damage. Temperature ree cfthe sample due ote elacvon Doan 8 ‘Sepencert on arumbe of fastors eluding accelerating volage and testy ofthe beam ‘cbservaton area, observation te, speofe heat and heat conaulMiy of Te sample, ard others Bolen mate anlr slogcel saris we geal Sscepl heat nd ay be ‘Garages Dermal byte electron beam. An cxample of ermal mage polymere ‘ater couse by tne election beams gven bet, . No beam carape Derage cue to beam raion Folowing are countermeasures avaiable fo beam damage, 1 Reduce the sample radiating current 2 Lower te accelerating votage '3. Apply metal costing tothe sample (to improve heat conduct), 4 Observe te sarpe whe cookng I @ Effect of disturbance FFingeso distortion appearing ona SEM image profle maybe caused by vibration oa say magnetic eld. Countermeasures for mage deturbance duet vibration are gven below {Keep ine Instrument wel away tom vatonsoutees sch at a-condona or pumps 2 Do otlethigh-vtlage cables Fam the column come in contac wh te wallor her iceaiation fame. {Dont tthe drat rom an as-condoner out contact the column recy, ‘Counteeasures for image disturbance de oa say magnetic fl area fllws 1. Keep the instrument well away fron magnet eld sources such as Wanstormer or lage tapacty power cates, 2 Shorten the working stance (ese 1-7 er 45in Chapter 6) and apply strong exctaton tothe ‘condncr ana sunt the eat oo magneto els 3, Use a magnetic fet cancel, Tage lesb vraiQore causes of image abnormalities Symptom Possible causes + Sample is not fixed in place adequately when ‘sampling + Screw of specimen holder is not tightened ‘Sample moves | adequately. + Sample is inserted incompletely onto specimen stage. + Compressor operated while the stage is locked. + Iradiating current is low (change the excitation ‘of condenser lens). + Lower image is being observed at short WD in the case of semi in-lens SEM + WDiis long in low vacuum SEM observation mode. Image fluctuates * Inadequate optical axis alignment Focus cannct | Objective aperture contaminated Crea 7 Recheck the instrument parameters,Chapter 5. SEM Instruments Available FE-SEM Lineup ‘sot March 2008 Ultrahigh-Resolution Field-Emission SEMs. Indens type FE-SEM Sem iniens type FE- (high vacuum) ‘SEM (high vacuum) High-Resolution SEM Semi in-ens type Schottky Outofens type Schottky SEM ‘SEM (high vacuum) (lowihigh vacuum)Hi-SEM Lineup ‘Scanning Electron Microscopes Em i. =m Out ot lone type SEM with thermionic gun Out-ofens type SEM with thermionic gun owihigh vacuum) (lowihigh vacuuen) ‘Seanning Electron Microscope bletop Microscope Outotlene type SEM with thermionic gun (lowihigh vacuum) (Wow vacuum)Chapter 6. Q&A for persons wanting to know more about the SEM! 41. Concerning formation of the electron beam 41) How isa fine electron beam formed? 2) How isa finer electron beam obtained? 3) Wat kinds of electron guns ae used inthe SEM? 4) What are the ciferences between the kinds of electron gure? '5) Whats the operating principle ofthe electron ens? 8) Whatis ions aberration? 7) What kinds of objective lenses are used inthe SEM? 2. Concerning evacuation 1) Why must the electron beam path be placed in a vacuum? 2) How i the evacuaton prtoemed? 3) What mets andor dements do the vacuum pups have? 4) What kind of maintenance do vacuum pumps equice? 3. Generation, detection and usage of SEM signals « +1) What happens when electrons strike the sample? 2), How ace backscaltered elections produced? 5) What kindof characterises do backscattered electrons possess? 4) How are backscattered electrons detected? 5) Wha the signal varying mechanism? 18) What are backscttored electrons used for? 7) How are secondary elocrons produced? 8) What kind of characteristics do secondary electrons possess? 9) How are secondary eloctrons datocted? 10) What ae secondary electrons used for? 49 4. Viewing conditions for acquiring good SEM images, 1) Whats a good SEM image? 2) What effect does accelerating voltage or condenser lens curent have on image quay? 3) How must accelerating veage be selected according tothe sample? 4) Whats the function ofthe objective lens aperture? 5) How does wotking distance (WD) affect mage qualy? 8) Whats astigmatism and how is it conectod? 7) Whats focal depth? 8) What isthe charge-up phenomenon? 8). How is sample surface potential changed by charge-up? 10) How is the image disturbed by charge-up? 11) What ae the advantages and disadvantages of sample coatng? 12) Wnat sample coating methods are avaiable and how do they afer? 19) Wats te pencipe ofthe magnetron sputerng metiod and plasma fim formation method?5. Principle and applications of low vacuum SEM. « 4) What kindof instruments the low vacuum SEM? 2) Wy is itthat an insulating material can be observed witout he charge-up phenomenon by means ofthe low vacuum SEM? '3) How is SEM signal detacton performed in the low vacuum SEM? '4) What are considered tobe the demerits ofthe low vacuum SEM? 5) Please ive a concrete example of application ofthe low vacuum SEM. 6. Generationidetection of x-rays and elemental analysis method 1) How aro xrays produced? 2) What kinds of characters rays ae there? 3) Are there any xaye other than the characeree ones produced by election beam radiation? 4) What is the extent of the area (depth, spread) in which charactriste xrays are produced? 5) What kind ofxay dtoctor is usedin the SEM? 6) The principle and instrument configuration for EOX 1) Whats the mutichannel pulse height analyzer? £8) The Principle and instument coniguation for WOX. 9) Whats the tandem type proportional counter used in WOX? 10) Are there any particular cautions to be observed in analysis using WOX? +11) What re the ciferences between EDX and WOX? 12) How is quantitative analysis performed? 60 7. How to improve accuracy in x-ray analysis ~ 89870 1) What shoul be observed in order to improve the accuracy in ay analysis? 2) How can characteristic x-rays be efciently producod? 3) What should be done inorder to avoid detecting x-rays prasuced from other than the ‘sample (location of interest)? 4) Isthere:a method for reducing the xray generation ares? 5), How doos the shape of the sample aflec the analytical accuran/? 18) What kindof pseudo peak appears in EOX? 17) What shouldbe done to achieve high-accuracy EDX ar ‘8. Principle and applications of STEM *~ 1) Whatknd of instrument isthe STEM? 2) What ae the characteristics ofthe STEM signal? 3) What features ae obtained by combining EDX analysis with te STEM? '4) Whats the method of preparing samples for STEM observatin/anaysis? 5) What are the appicatons of STEM (EDX)?|. Concerning formation of the electron beam inthe usual SEM instrument he elton LY4 source (ameter) formed by the eecton aan recto gun (See in chapter) reduced and made int a fine electron beam (ameter) by the ‘condenser lens and objecve en a nated in Faq.1. The condenser and objective lenses of 4, the SEM ae bot leromagnetc lenses (1-8) ‘The magnicaion M, Ma (or eduction tein ‘SEM ofthese lenses is expressed by My = bes, ‘Ma = bala, and the final beam diameter is dy ane comet ert ‘Athough it would seem hat cout be mae, infil smal by reducing My and Mts not ute that simple. Ft ofall, ye shortened land M, reduced excessive the etectrons incon onthe bjecive lens willbe reduced and probe cuent (eracatng cure required for formation ofan image wil not be obtained (208 Fa.) Actually he condenserlenscurrentis PB. SchemeferOBiahing aire Becton Sean adjusted so tat My wil be minimized inthe range ‘where a sutcient probe current canbe obtained (42). Also, since image distortion caused by lens _berraton wil be aided (1-6), theres ait tothe reducton of, Note that «hers represen ‘opening angle othe electron bean (15). he Wor ‘lanes (WD) 2) How can we obtain an even finer electron beam? In xd ocbiain a ire elecon beam inthe SEM, te nstumentulizes an electron gun featuring a smal electron source, a large current densty (curentn Alem’) per unt area), anda smal energy wisn (energy vriaton (eV) of ischarged electrons, plus an objective lens havng very te aberration. S00 (1-4) and (1-7) for mere detas onthe characteristics ofthe clacton gun and objective lens. Flowing are points to keep in mind when sting te viewing conten. 1) Adjust the condenser lens cuentappropritely as mentoned on (1-1), 2) Use the objcive ons atthe shortest possible werkng distance (ND)(-7, 48) 5) Set an appropriate bore diameter forthe objective lens aperture in order fo minimize lens aberaton s), 4) Soce he emiaion currant decreases witha lower accelerating voltage in 2 SEM using a themionic source (1-3), cary out flament height agustment and bias agustment to obtain the desird curent 5) Be sure to cay out astgmatism correction (8), a{3} What kinds of electron guns are used in the SEM? “Tneeionio ype gun (ungstn han type, antrum nexaboride (LAB) type), fet emission (FE) ‘bun and Schottky type gun are generaly used inthe SEM, Figuo2isates te configuration and prince of electron emission foreach type of gun. Electron emissions achieved in respective cases by appling thermal excitation (applying energy o electrons while nesting) by using 2 tunvel eect, (forcing econ out ofan energy barr va‘a strong electric Hl), and by using the Schothy fect ‘lowering te energy bari by means of song elec el), with which conduction eecrans in ‘metal can overcome the anergy bari exstng at he boundary of metal and vacuum ‘Tungsten diatent Rioeleration power ply 9) Termionc gun tungsten hain ype) Tungsten s neste and energy is Lanthanum bexaboride (La) having 2 applied o canductonelactensin ‘smal work function (lectons ae ‘order to overcome te energy barrier ‘easly emt) is used instead of ‘at metaizcaum boundary tungsten Flashing power UPBIY —petacton Suppressor me Heating poner power ly -Butlor type anode ©) field FE) elscron aun « Sehote election aun ‘Astong elec feld x concentrated on | | Tips enated wih ZrO, a strong electric the tp of tungsten single ys, and ‘lis applied while heating and enesy ‘energy bares narowed and electrons | | bares lowered via Schott eect 0 forcod out va the tunnel fect. cent electrons. Fig.2. Confguration and Principle of Eleton Eistion with Various SEM Etecron Guns Ey4) What are the diferences between the kinds ofelectron guns? “Table 1 compares the characters of the tungsten harp ype thermionic gun, LaB thermionic gun, and FE and Schotky electron guns. Important factor inthe femation ofa fr elacton beam: sre electron sure date, brightness and energy wath, andthe FE gun excesn a of these ‘characteris, tus fing wide use in high-esolion SEMs. As @ universal ype of elecon gun, ‘the tungsten harp type theronic gun operates wit) a relatively simple evacuation system and [provides @ lage probe current, ands spplcabe to a wide range of wes trom low vacuum SEM (5-1) ‘upto EPMA (6-4). The Schottky guns sight infarr to the FE gun in electron source amet, Dbeghiness and energy wish while roving aarge probe curent and is applicable to a ‘mult-functonal hgh esoluten SEM feating high esoluton observation lus xray analy uncon 65,58) ‘Table 1 Comparison of Characteristics of SEM Electron Guns aE open fe a Tungsten single pten | hecaore ng seston | crystals material sults) crystal oxide Catan wo |e 120 | fooinop, | 2700 300 Rathode work a 261027 a 27929 Mar re 1 a 108 10 Weskne 10 7 oe oe sth Meus | ~0 100 —| yaar ormare[—~Somii5) What is the configuration andlor operating principle ofthe electron lens? Electron lenses inde magnet field ons and elocbosaic ns, andthe description hee covers the magnet field ers thats generaly empoyed inthe SEM, The magnetic fei lens serves to {focus the elacton beam formed by the electron gun (1-3) int @ fe probe and race tonto the sample surtace, andthe SEM uilzes one or wo condenser lenses and an objective lan fortis purpose. The contguration and operating principe of he condenser and objective lanses in tbe SEM ‘18 shown inFig. 3. “The clcron boar incident on these lenses ssid by the magni fl produced tough the ‘92 (p0-pece) nthe magnetic ath, Is converged while rotating around the optcal xis, an forms a reduced image of te eam onthe image plane. Note tat the cbective lens is designed 0 8 nt to Intror with samplemovernent or secontary election, ay ‘signal dtecton (37,65). ‘This acon is expicined in futher detain Fig 4 The ectonsemited from each pont ofthe electron beamare focused ont the corasponcing image ont by the elector lens and form areduced image of the beam onthe image ane. The redueton rate Mat ste is expressed by M = (1-1. “The reduced image rm the ‘condenser lene becomes the beam forthe object lens, and ‘he reduced image om the ‘objective ensiseradated onto the sample Noto thatthe reduces image ‘nets some sistorton caused by lens sberaton (18). The aperture ange «is determined geometrically tom arene ameter ofthe lens re ameter of aperture) ana focal stance, and ha a ego Influence on lens eractorits such a lane aberration and focal opth which willbe explain ator (4) Fig. 3 Contguraton and Functon of Eleton Lens ‘Gedued rage) Fig, Reduction of Eicon Beam by Magnetic Fil Ler u6) What is lons aberration? Lens aberratons many incude spherical abortion, chromatic aberration, dracon and ‘stgmatom (4-8), among which itis iffcut fo completly exclude astigmatism, tis heetore recommended o cary out observaton under condton in which these aberrations are minimized in ‘tet obtain good SEM images. 2 Sobral aberaton ° i ‘Spherical abortion. 38 shown nF, 8) peeled ‘sa dtrion caved by a cference n a coment postiratsieen secs ssn are lon coier aa leone passing ataoaton eva tom te cater, fe exe os orn de reprint the cab of pening ange. Obed lene Gis teepterealaneraton coca ang ATMS oo}fe-Miniumbr cle be stoner foal tars (1), e120 sneterne cso! beraton cn ths be edices by ua a smal ape bore santa ac ano os ites 3) Chama baraton roma teratn,aindated Fa $0) incase avaratonin ena (vavengt)oflerons ent onthe lone aeons Soon proportion ener variation GE are ‘opting angle 8th coma Sheraton orice an tacomes ser se cal tance becomes sot Ciromat seraten can are be rece by deceaing the oer with of soc beam (14) Unga shat cal tance and reducing the opening al “Tne eet cfcromat aeration sar «5th acasratng votage becomes ower )Diracton Dracten as tstatain Fi Se) 8 arracon of encvons casey eating tne coment ang beam opening olen) fees ansiteaisesihe Fg S Genaaton otters Abotens an Tat eam widen. Theexentof tis) Spaealaberatn, 0) Cemate aeration) Diacen aeration 8 proportional the wavsongt fearon andin ives proparten pening angle Alncigh ean bereieas ty meres aertre dameter. he steral and conte aeraton wilinrease, she secure sanatermustrtbe enue oo mich 36‘T)What kinds of objective lansas are usad in the SEM? Spherical and chromate aberations othe obecvelns become smaller by shortening the focal distance So in action othe ou otene ‘ype of objective ans general used withthe) iecton beam SEM, an nons type having a shor for rere gh-esoition SEMs and a snorkel ype (or semi inens type) have been developed. {2 Outotens type objec ens islers asideatedinFg cae | Sea Wi lee as nated Fi. “dary Def aii, ‘valli fomed at potion stove the coeur pence sample, sothare is a iit on how mc fan BEBE 8 eaten be shoteed. Athough his make raher Lnsutabie fora hghzesouon SEM, tis Semple eae convenient for cbservatin of large samp Sree large working dance (WO; estance from loner face offers pole-fece to suface of) sample) can be prvided. Ths lens Secondary _2pplicatieo a mutiunctonal SEM sinceit let parmtsobservatonanaiyes of magnet ‘ater with whic leakage magni ks ‘round the sample is sma »)Inens ype objective lens “The feature of thi en, 38 naa in Pg 60), shat canbe extremely shortened because a sample is laced inthe gop between upper and ower pole-pleces. I's therefore applicable to utahighresluton SEM, but theresa it on sample ze and itis Lnsutable for observing stongly magaetle matoral Secondary electrons are spun "par by the tong magnetic fed ofthe lens and detected by an SE detector mounted _bove te excting cal an ens. ©) Shore! (som inten) type objective lens wh the snorkel type en, aiid in Fig 69), a pole-pece gap is formed an by bringing the vtual lens lose tothe sample, ange lecton beam samples canbe observed ata shor (+ WO), Fig.6 Kinds of Objective Lenses Usedin SEM ‘Secondary electrons ae detected bythe unper SE 2) Outotens type, b) nies type, detector whan Tis stor, or by he ower SE 6) Snorkel sem ine) type detector when fi ong a2. Concerning Evacuation “4) Why must the electron beam path be placed in a vacuum? IFelectone wee to encounter number ofa molecule on their way toward the sample, hey ‘woul colle wah those molecules an seater, whereby they would not reach he sample. To avold ‘seh a aston the sac haar path the SEM etna kept ina warm th hin ie ‘molecules are minimized. The distance over whicn an electon vances ater once colicrg wih 2 catain molecule untl the next cision i called the “average foo moton of the elector, and by reducing the pressure and extending this meson as far as possible, the electron can reach the sample witout contacting an ar molecule. The eleevon beam path of he SEM Is generally Kept st 2 pressure of around 10° Pa, whereby the average fee moton of te electro Is abut 40 m. 2) How Is the evacuation performed? ‘Atypical evacuation system forthe SEM is shown in Fig. 1. With a SEMRavng thermionic gun, the entre election beam pat rom electon gun to specimen chamber i evacuated by al dtsion pump (OOP) or urbo melecular pump (TMP), and manisined at pressurect 10° 10" Pa. An oll rotary pump (ORP) is ulized for pre-evacuation at specimen exchange or fe post evacuation in oder tokeep te backxessure of ODP/TMP on. AS forthe electron gun chamtsr ofthe fed emission ype SEM, kmust be evacusted on uahigh vacuum of around 10" Pa tc kep the surace of the ‘lecron source lean at an atomic level. Asputerion pump (SIP is used orth purpose. Noto ‘athe electron beam path contains a number of smal paritoned comparnents connects by ‘means of ones, anda aiferental evacuation mechanism suze for gratualy increasing te pressure toward he specimen chamber This enables keeping the electron gun pressure constant ‘even ifthe specimen chamber pressure varies. ‘Altough te specimen chamber is evacuated by ODP or TMP the same s wth the thermion type ‘SEM, @ dy pump such as seo pump may sometimes be used In place of ORP for evacuaton of he specimen exchange chamber or postevacuaton. The reason fr hiss tominimze the effec of ‘specimen contamination caused by backstveaing of of vapo from ORP, SIP ORP(OM Rotary Purp) (00 (0% Dison Puno) ontin [8 SP TMP(Turbo Molecular Puro) ‘SP (Sputter ln Pare) etaSenee = chamber 4) ORP or dey one we oppor tmp Pump 1) Thermionictype SEM) Fal emission SEM Fig. 1. Example of SEM Evacuation System3) What are the merits and demerits of each type of vacuum pump? “abl gies he operating pressure and merts or demerts ofthe main vacuum pups. ‘Table 1_ Operating Pressure and Meris/Demerts of Vacuum Pumps Kad el pap | Operating ents Demers pressure a) ‘ORP ‘Aimoaphor |“ Usabio or pr-evacuaion | “ Uneuale or ole pressure to | (atmos phere pressure) sopicaton io" «Simpl sete ons + Foor aon is ater ge lowprced ‘Dry pump | Aimosphori |= Usabieforpre-evacuaton | » Suuclure is rater conglox ard (saat pump | pressure to | (atmos phone prossize) highprced, ee) io + Oe evacuston ‘OP 109107 | + Rapid evacuation = Some dapersion of olvapar “Notness orvibaton causea | Remuites pre-and postevacuation routes water hier THe 10" 10 | -Oires evacuaton Complex stucture ard “Wide range or opening orem pressure + Roqutes pre-and poatevacuation oF TO"e TO" | -Nomechancal vation | - Evacuation ate ow “towsowerconsumoton | + Roquves pre-evatuaion 4) What kind of maintenance do vacuum pumps require? “The ORP pump ques olexchange onoe every si month oa year, o be criod out by the user Exchange shouldbe prfrmad using the ol and mathe prserbed in the Insbucten manual fr te ur. though ether pes of pumps have almest no maintanance tobe cared out by the user, fozow the pump nstructen manual as o frequency of periodical hspecton specie bythe manufacturer 8‘3. Generation, detection and usage of SEM signals 1) what nappens when electrons strike the sample” ‘An electons very smal n comparison ‘wah the space between te atoms which ‘compose. specimen. Therefore, when cident clocton ‘an electron penetrates the specimen Xray ea catered tough teractions wit the aan ecary ‘toms. Inia process, some ofthe eee sloctron, incident electons fy back into vacuum as ackecatleed alactone (208 2) Fg 2), butothers lose energy whe emsting_Cathodaluminessence secondary electrons Fig 3) ays Fig 3), Fgh (cathode uminescence), et. and finaly remain inside the specimen 25 Specimen showninFig. 1. Incase ofa conducive fabrarbed specimen, te primary electrons remaining inside the specimen are etected as specimen (absorbed) curent “The eeciron dispersion inside a Fg. 1 Inleracton between Inset Electrons specimen can te wauakized by the ‘2nd Specimen technique of Moate Cari simulaton. An example ofthis visvaization is shown in Fg.2. This example reveals that he Incident elecwons are dspersed over a er area when tec energy is higher and he specinen densi sate, Soscimen ,scidest electron pnetenson aren » @ oy ‘20am 4 2c 29m O2um Fig. 2 Electon Scatenng inside Specimen as Visualzed by Monte Care Smulaton {3} Upon inccence of BV on carbon (c) specimen »)- Upon inedence oft keV on carton () specimen ©) Upon incidence of 15 keV en gold (A specimen 382) How are backscattered electrons produced” ‘Backscatered stectrons (aso caled rected eaters) are ven bith inthe folowing process. ‘The etc incdont ona specimen cause |Rracions wih te consttuent alors of he specimen {pa are scatred backward into ie vacuum, orn the (Srecton oppose othe Beam as shown INFg. 3. Eocton starter n a specimen are cassiied ino 2 ‘ypes: one elastic satorng whi nent ‘ctons are scared ata large angle wth almost no lessin energy, and he others noaste scaring | ‘ates inogent lactone loose onary But are Soatored ata small angle. Asa Ypral nelastic Seaton, we know the emscon process of ‘Secondary election and characertle x3. "The esmtealy scared eacons Paving ‘apron the same energy athe nedont ‘lecvons are scatered rom Be vec of specimen Seas nie cui, wa be tay ‘Seatored electrons which have ost ene Aton (Characteristic xray ‘Xtc ar scares om a compart eep lceatonin the specimen tote vacuum These Fig. 3 Seating of nent Electrons ide lctors ar collectively cae backscattered a ‘lots (reected electors). 3) What kind of characteristics do backscattered electrons pessess? ‘The cunt ayo hacaered elon ‘tw olecens incident on specmensurace i Caled alc rfectviy" Actange In “tis retctiy renders a contrast 0 backscatered electron image. Figure 4 ‘Shows diferences in econ refieciy famong same specmens.iscbvious hat ths refocy value becomes lxger asthe ‘mean atzmc number (or dons) ot Speamon nereases. Thus, backscatred ‘ecto signal covers the contrast which Fett he specimen composton, tis Considered tat his signal proves Inormaen about ne companion appld detector (35), Summarizes here each structure and characterise ofthe YAG an eomiconauctor detectors 2) YAG detector ‘YAG detector uses 2 YAG (ium Aluminum Game) cyst forthe scntiat, wih wich phosphorescence generated dus o entrance of beckecatared econ lect the ghatomutipl| (PMTy@-9) wih the ight guide. ARorr-conversion int electrons, amplfieation i made oobi @ sonal curent “This cetctc has fetues suchas compat with image observation at ahigh scan speed because of is high response speed, usability over abroad range of accelerating voles, et. However ts cfu to use this detector fr 4 Necessary infomation a given Below i leaty exqresse. “Topographic fermation, compositional formation, cyst nformation -<2> Wrong infomation as gven below i ot cotsned \arousarfacs, damage, external istunance te Gradaton and brightness level are appropiate 2} What effect does accelerating voltage or condenser lens current have on image quality? (changing the accelerating votage ater be inedent ‘lecton energy to a specimen. ‘This entas changes of lns ‘elaioaip betwee Acleaie Village on Tne Quality ‘aberration (1-8), aes of Hams elated toiageguity ‘dlecton seating in the Timage inrmation ‘specimen (9-1), secondary ape largely on peeines) ‘eeeton emission yield (3-2), nae rseation 26. Inconsequence, various _epedelarely 0 oncinen) Image quay changes 2s shown In Pig. + are brought about “Therefore, accelerating votage ‘sone ofthe important operating parameters or obtaning @ good Chery ‘SEM image. Theimage avaity ae changes sted in Fig 1 depend) aren are. on acinen) Conese High x largely onthe substance and shape ofa specmmen. S0YOU Emison ofharetrixtex ay should se this figure for Fig. 1 Relatonsip btwoen Aoceleraing Vatage Change reference ony, (Change oa terent ‘2 image Quality in SEM condense exctaon curent ‘ters the focal lenge (-8) of (Teanga ois Quali When Vain Condens Lane Cit thisiens The ents changes of probe curent and probe am amet (eleron beam Si dlneter) Inconsequence. tne Muimbement and ints Seat OC Large curertconsions of age pepe = resouton SN rato, chageup SENSE EE ru (eantonone carae vl TSE” Laces Saat FE-SEM (1-3), the probe a Wil ee o— diameter ca be sid tbo fess SHEEP neck teat steed by change of he Seis ee congerserlens curent nana Speen damage serious Skt ‘eminic emission SEM (ap, Sepsis eon sss) because the electron source ‘Fg, 2 Change of mage Quality due to Condenser Curent dloreter of FE-SEM fs smaller Adstnent 03) How must accelerating voltage be selected according tothe sample? ‘Contrast ofa secondary slectron images dependent signicenty onthe shape, deny, te. of specimen. The stuctues of buk specimens for SEM ar oughly classfiabla ine 6 catogores shown In Fig. 38) 0. For eac category, an acceleratag valage which canbe thought fo be aperopriat in general's described. However, tenon shouldbe paid because an appropriate accelerating wotage ‘ters depending on te cbject of cbservation (desired kindof information) even among the specmens of the same structure. Not thatthe ow accelerating votage, medium accelerating volage and high accelerating votage dasccbes hare stand or 2 KV or ower, 3 to 15 KV and 16 KV or higher, respective Fig 3 8 ad p dnote secondary electron emisson ye an specimen density, respecvly. However, charge-up (4-8 04-10) occurs because ofan eectcaly non-conductive specimen, ving ata low accelerating voltage of + KY ess or pelinary eating process (411) to 413) kroquod regarless of specimen structure Fg. 3a) For vewing a high-lnsty parle, et. on low-density substrate ‘SEM is most-uted fer tis kind of specimen, Because he quently of SE i larger han 'SE2 9nd SE3, highesouton imaging it possible Partles or he ike can be observed athe high accelerating voltage though the fre structs ‘on he surace ofa aubetrate can be beter mage a the iow accelerating votage. Fg. 20) For viewing 2 low-ensty pate et. on high-density substrate ‘SEt and SE2 produced rom the subseat cluding SE are more than those due to parties, tc. Therefore, ne particles, te. cause black contrast in general. Thelow accelerating ‘voltage issuable for viewing he parle, ec, but the surface structure of he subst sf can be maged at a wie range of accelerating vlages. Fig 30) For viewing high-density partes, te. us below the surface of low. densty substrate ‘SE1 and SE2 emision snot so expectable. Depending onthe infomation brought by SES at the mediuniigh accelerating votage, the paces, ec nthe specimen canbe ewe However, fr vewing te surface stuture ofthe substrate tse, tn ow accelerating votage ie beter Fl, 38) For viewing a low-donsty particle, et just below the surface of Nigh dena substrate Its atc to view he particles, et. doc fom the surtace. Coss-sectoal cbsevaton 's required. Howover, the surface topography ofthe subsrato tse can be vowed at a wie ange of accelerating votages. Fig. 26) Forewing fe topography of low-density substrate surface direct wihout coating ‘Because the incident lacrons are scattered wisely Insite a specimen, viewing at Ne low acocleraing votage is unavoidable, Fg. 39 For viewing the costed tine topographic features on the surface of ow-densy avbette Sine the informations mainy sen ftom highest coate fim, viewing is alowed at wide range of accelerating votages.ee a Paface tis fim EBal pio + Pail, chin Say structure Mein to high accelerating fectoningrequied voltages + substate alae structure + Subetrte mrface structure ‘Mie ange of acelorting Siow acoslerating vltege votages ° ® ee SEIN | Conte fim + Subsrate murface strusture + Subetrate aurlace structure Ee eceeree ied SNieetinee acer: 8 Fig. 2 Various Specmen Sutures and Aceslerting Votage Seting Suite for thr 34) Whatis the function ofthe objective lens aperture? The abject lone apr cont the civergece an (15) ot eevon beam fd the rumba of ecb (probe caren pass tvough&, and acs he | Aperture be sine ecton beam dame: (wsluton fecal Variable factor and ta ep (7), mage SN rato, as fence cwerimage | Smell Stare thowninFig.4 Forebisinngthe (Beam dlametar | Optiman: ale erating trinimam decor beam deter, priseasare ol aerreore et eptinum aperze se neds tobe selected gee The opt size ves wihSEM. Sorterercestousne Image SINrato | Low ich trade ote induction manal of ach SEM. Forempovngimage SN toby Fg. 4. Functions of Objectve Lee and is Intuence inreang he probe cen ager cer image Guat, pene regeed, and a saler spare eqvedforineeasng he ‘eal dom, ‘Objective Lens Aperture Bore Sil Influence over image Quality Focal depth Deep Shallow 5) How does working distance (WD) affect image quality? Changing the werking ditance (WD, 4-7) brings about changes inthe focal length of abject len andthe own vergence anal (1) of lacton Variable factor and its beam. Extending ie WD eniarges EMS OEE ‘he diameter of eleton bean, but Focal en icraues foal depth (7), Ako, when ne feed) hon the WD is extended, the citation axength of ‘Working Distance’ Infaencn over Image Quality ‘scanning area of SEM widens and eee) magniteaton decreases. However, Electron beam agniiation He Blectro this does not cause any inconvenience in practice because amodem SEM Magnification automaticaly corects magnicaton by peat depth detecting the objetvelenscurert kr COnthe cher hand theinfuence by «fogtngmauetic | Small Large eating magnetic field (AC S080 Hz, Sl DC magnet el, ec )s00 Chapter 4) becomes ager athe WO is extended ‘ad image roubles may arse ‘Therefore, you should be caret about Wo extension in igh-magrifeatin cbservtion Increased Reduced (aly aus section works) Shalbw Deep Fig 5 WO Change’ ntuence ove Image Quality'6) What is astigmatism and how is i corrected? ‘Astigmatism refers tothe bluring of nimage which occurs when he focal pint ff an electron passing trough the X axe of lee i leven! rom the focal point yf an electon passing trough ‘he Yaxis. Thisis caused by an asymmetrical magnetic ld due to misaigned electron opts, charge-up obenomenen due to contamination of he electron Beam path, eas shown in Fi 6 ‘Therefoe, when astigmatism has occurred, the cross sectona shape of lcron beam at isan lps lng in the vertical recon because focus is atsned in the X recon alone, ad that ts “an line longin the horizontal crection. At the correct focal pont (alo called "ast ec of confusion” 1-5) betwoon andy the coss section has.a shape ofa complete ce, tut fine ‘locton beam is unoblainable because fous i attained a tis pintin nether norY direction ‘actualy. Hence, astigmatism corectons requed. For ths purpose, each curren ofthe X and Y ‘aslgmatem corecton cols adjusted so that andy match fn actualy, astigmatism doesnot ‘always match the XorY ax |e, eccusin random drection, but astigmatm ina random ‘Srecton i corectate by ajusing the vector quantity ofthe XY magnetic els neath corecton col Fig.6 Astigmatism and ts Coecion Method Figures 7a) andb) show images at i and fy under presence of asigmatsm. Because the electon beam seit, image stretching has occured. Sretchng rections at x and y are GO ferent tom each alter Phot.) shows an image atte. Athaugh image seething id nat appear the ‘ontroimage's blued. So, the curentof each astigmatism corecton col was adjusted 303810 ‘obtain the sharpest mage posable. The resutis shown in). Now t appears tha asigmatism ‘correction hasbeen completed Bu, when magnification was increased, During becomes ‘onsplevous again 3s shown i). So, sdustment was repeated so as to make the image sharpest tf, andthe imapoin photo) was abained. Sy confrming the aetgmatem ovecton a ‘magnicaton two o thee times as high a he photographing magnifeaton nthe above-nenvened ‘way, complete corecton can be made. isFig.7 Astigmatism Correcting Procedure (specimen: inner wal fas rachea) 2),b): Under presence of astigmatm. mage stretching is observable at and, ‘and is dracon 90° decent between the two pins 1 Atfebemeen tend 1, ne image s ued, out sttching not obsevacie {9} Atf, the satgmatem corecton knob ie manipulated so tat he mage becomes the sharpest. AS a result this image can be obtained. When magniteation is nereased, luring Becomes vibe again. This sgrifes| ‘hat astigmatism coreion sna completed. ‘Repeat astiatem corecton, and he sharp image wil be formes ueA wnatis focal depth? Focal dept Drees to diane ragein te recon ot ht were nro specs (aoe hclend aren wen fea pot ts devated ue tothe Sofas unevenness fhe mage Ss shonn nF 8. Ths ph i termed he deraence Angin 20 elon De and te renrn ean ecto mM fonenimoge incase of SEM Blecton box Divergence angle 2a ise aie Mon specimen, eT Focal depth D Specimen, ‘the minimum size corresponds to ‘he pis sz SM on 2 specimen, = 28a Terr lw con u display * 1 Magnification D=254M ‘where, nd M stand forthe ‘piel ize on display (or Fig. 8. Focal Deptin SEM ‘photograph an a magniicton, ‘reopectly Thc cigrifles that he focal depth of SEM ie longer when te ez of he objective lone ‘aperture (4-2) smal, the working distance (WO)(45) is longer and magnification is ower AS ‘agnfcaton nreases, the pl se SM on a specimen becomes smaler_ So, beyond acetan ‘maghifeation (usualy, afew tn thousand tines), the elecvon beam spotoveiapsneghborng pines. Insuch a conten the electron beam diameter can be tought asthe mrimum recognizable size Instead of the pel size 3. '8) What isthe charge-up phenomenon? Charge-upie a phenomenen where te negate charge of he ner electron beam accumuites charged up) onthe surfece of @ non-conductive seecimen ans the potential he beamincient area changes to cause various imege troubles. ‘The chrge-v phenemenon curs when the total numberof elton emit from & speomen or beckscteres eecvons i). boobed eecons (a) and secondary electrons (a) not equal oe namie of Incident eectons(), 28 stom Fig 8 "The potential on specimen siace becomes negative whe a> hx * ‘And, becomes postive when Is lee * le Incase ofa non-conductive specie, ln Is almost 200 and isis termine by the specimen ouixionoe, Three, the Fo. Charge-up Phenomenon on Suace andy ofl, namely seconcary electron rae erission yi (9-8) determines the chargeupstuaton 55'9) How is sample surface potential changed by charge-up? charge-up occurs, the potrial onthe specimen surface changes toward the postive or negative 140 unt the secondary electron emigson yield basomer 1 shown in Fg. 10. Therefore, the lev! of specen surface potenti may be approximated by te erence between the atl incident ‘lection energy and the incident electron energy where 6 equals ton the observed specimen. However the nesent electron energy where 5 equals varie with specimen and imaging condos, Inthe example shown in Fg 10, tis probable that he potential changes about 800 V toward he postive se wen the incident energy I 100 eV and cose to 9 KV toward the negative side when be ‘eneray i 10eV. However, the suace potent snot lvays constant in actual cases, because this potent may be sigifcanty ferent locally due to # complicated specen profile or chargnglaichargng may be repeated at covan intra. Fig. 10. Chango in Specimen Sutace Potential at Occurence of charge-up 410) How isthe image disturbed by charge-up? ‘And, how can the image disturbance be prevented? Image toubles due to charge-up phenomencn can be sried ito to fypes;<1> mage csturoance and <2> abnormal contrast. Ther are cases where both types and <2> neve Type <> ‘occurs a shown in Fi. 11a) because te rata positon of nent electron beam changes, sifected by an electri ld caused by charge-up. This disturbance rises when the specimen surface ischargod up at acomparatel igh potent. For preventing this disturbance, reducton of the probe current as shown in Fi. 11), lowering ote accelerating voage, et. are efectve. Type “<2 ccus as shown in Fig. 128) because secondary electron emission i aected by the chage-up ‘lotic Fld. In case ofa postive potental the emitted secondary electrons are pulled back the ‘specimen site and cannot each the detector, co a bck ze appears. Incase ofa negative potential a white zone appears. Preventive measure is bascally the same asin <1». In Fig. 12),‘abnormal contvast has most been suppressed by educg the accelerating volage 100.7 KV. ‘Aunough some land eror process necessary because he secondary elton emission yd (@-8) vais wih specimen substance and maging conations, t's general though thatthe charge-up phenomenon canbe suppressed sutstaniaywiin an accelerating wolage range from 25 10 KV. However ifthe charge-up phenomenon cant be prevented by changing the probe cure ‘2 accaleratingvotago, then its requtes to vacuum-coat a specimen (11) ovew tin alow vacuum (6-2). Fig. 11 Example of mage Disturbance due tc Charge-p (Polo at rahe current 20 pA fora}. ? ne ‘Accelerating voltage: 7K ‘Specimen: lulls on inner walofrs sma irtestine Fi 12. Example of Abnormal Contrast due fo Charge-up (Pho bt ‘Accelerating voltage: 1.5 HV fo a, 07 KV for) Probe curent About 1 A Specs. Resa ptt11) What are the advantages and disadvantages of sample coating? Sampo coxing i intended to provet ne charge-up phenomenon by afowing the charge on the specimersurace go to ground through he coated conductive fim as shown in ig. 13. Besides, specimen coating has advantages, or ‘example, damage o the specimen under servation can be reduced because thermal conductivity isimproved, and the quanty of secondary earn sgnalincreates (On the ote han, specimen coating has Alssdvantages, for example, the shape and sizeof _ananometaroderfne structure may changs, and "specimen iformaton abou elemental ‘composition and surface potential may bel. “Therefor, is requtad to select an appropriate ‘eating meted according to the object and Pec ‘Buose of SEM imaging or aves coating in aaich Osis undesrable cases. 412) What sample coating methods are available and how do they difer? “Te generaly empioyed ceatng methods listed in Table 1. Armang the metods, those frequent used for high-resoldion SE image ctservaton are magneton sputring and pasa epostion methods. However, ary method sues for observaten of low-mageicaton images alone, and the resistance heating method is used in carbon coating fore ray analy ‘Table 1_SEM Specimon Coating Methods and their Characterstes Supplement43) What isthe principle of the magnetron sputtering ‘method and plasma deposition method? Te magneton srutering method is a ind ofion sputtering metnod, but has 2 permanent magnet ner the sget. This ‘athed werks on he allowing price Fst, the elecrons accelerated by an ‘let fla between the target and anode inthe Ar gas atmosrhere 1-1 -10Pa) coli wih the Arges molecules to oie them as shown in Fg 14. In tis process, ‘he electrons move dynamical due to don ofthe magna el, which increases the probabity of eoison ‘Therefore, movement at alow votage is 2 Srecimen characteristic of his process. The resutant Fig. 14 Principle of Magnetron ‘Arions are accelerated byte elect Sputtering Method and it gaint the target platinum P), and ‘he Pt paricles are gjcted out ofthe target ina sputorng phenemanon. The parties are accumulated onthe specimen surface to fom a coating fim. Since the magnetron puting method works ata ow voage, redveton of specimen damage and ‘enhancement of fimthickness contotabilly can bo expected. “The osmium pasra deposition method is based on he folowing prince. Plasma 0804 -» OF" + 204 46 <2 OS" +e + 08 Fg. 18. Peneiple of Osmium Plasma Depostion By tis method, an amorphous and dense Maho Osfimis obtainable Also, he elecrode ‘suture has been inproved for reucing ‘specimen damage, s0 discharge at a votage ‘98 ow as 600 V hasbeen realizes, ove Fass ade Zore| meaaske hs sid Helow Q cathode [specimen s5. Principle and applications of low vacuum SEM. 41) What kind of instrument isthe low vacuum SEM? ‘Low vacuum SEM @ SEM which can be operated at higher specinen chamber pressure (ower ‘vacuum condton}than general SEMs. The specimen chamber pressure na general SEM i kept \witin10° to 10* Pa, while the pressure alow vacuum SEM is kept at a much higher presse, or @ few to several hunred Pa. Operation at high specimen chamber pressure enables electron ‘mcrosopists to view a non-conductive specimen quel ina nondestructive way omiting a step of _peeimen preparation and also suppress vapeizaton of moisture and olin a specmen dureg ‘observation. Not that amos al the commercial low vacuum SEM are aso usable a8 general high ‘vacuum SEM twcugh cnangeover ote evacuation system, 2) Why is it that an insulating matorial can be observed without the charge-up phenomenon by means of the low vacuum SEM? men 8 non-conductive specimen ie wed wih a general SEM (igh vacuum SEM), mage rouble may Table 1_ ean Fre Path of Electron (in Ns gas) oozur due to ehage-up phenamanan Speen GEE | Nantes path (48) to disable normal vewing. For oe aa ‘ereurventing ti, the specimen ‘surface usualy coated wit atin Pa, ie Sa fir of metal (412), 4-19). However, 210Pa ‘Alsat Oe coating invovesimpating of the orginal specmin characistis, wien may ead toa ind of destructive observation Forsuch winerable specimens, @ low vacuum SEM Ws ofetve. Ata high specnen chamber pressure, be mean re path ofan electron (2-1) short (se Table 1), and he psnary ‘lector, secondary elecvon and beckscattredelecton code withthe residual gas to jnize thom as shown JnFg. 1. The postive ons esuting ‘rom the nization move, tracted by the negative charge accumulated on ‘he specimen surface and nevtalize Fig. 1 Suppression of argo ‘he charge. inthis mecnansm, alow Phenomenon in Low Vacuum Enon ‘vacuum SEM superesses the charge-up phenomenon to alow crt ‘observation of non-conductive specimens6, Generationidetection of xrays and 1) How aro xsays produced? \en an neidenteeton ets an otta electen ina specmen composing atomin he process of elas seating (3-2), the stom assumes on ext sate (is nized). Then, anslecton Is ‘ought fom an outer elacton oti th vacant ne medio seen the stacy sits ag8n aeshown Fg. 1. This phonomenan scaled a ranston” An excess energy produ in tis proces of econ ranstonis feted a8 an xray, Because trecterencenenesy betoon testared ston two atts aes ona vaie unique ore element the enray of me omit ys aso unique tothecloment. Hens, this vray cals a characterte cay wh sued foe ‘omental aay. For ‘generating especie character ray, an econ saving a ger energy than hat ofthe rarer xray nods tobe projects. Notethat he ‘eatensip vetwoen every E (eV) and wavlenath (nm) can be evproste byte flowing eatin = 123.90. Incident electron Characters {Gevtng an ener peculiar to demend Fig. Generaton of Characteristic X-ray in Sasiun (Na) ‘Atom Mode! 2) What hinds of characteristic xrays are there? ‘There ao many characinste xrays * ve to aierence ne eneray y eveen thers where an elcien NSH ‘ransiion (6-1) occurs. Typical ones t ‘xe shown inFig. 2 Forexarple, characterise xrays generated upon x fronston fom te Lok MEK OR a6 it a om My © Kare cae Kay near ' Gy Ine Anda pi of Kay nd oy oes anda of Kandi ines maybe : cobezivey catea"Kains nd shal Ines respectively ora par of and 4 Ines maybe clea" LorMines” Kabel ‘Among te characte xrays ofeach 98 BB GBP OB ‘ement the Kies have te largest Kline Lines" M ines energy flowed by he L nes, and M Fig. Typical Charateriste Xays and ther Names Ines in tis cer «63) Are there any x-rays other than the characteristic ones produced by electron beam irradiation? Figure 3 shows te characteristic ray spectrum ofa tines steel specimen which was measured wen an eneray-clspersve xy spectrometer (6), Characters xrays are dspayed as _smal-vith peat, ena when the central energy of each peak can be detormined the element contin in the specimen can be kxown, On the other han, this spettum contains the background Just resembing he back of whale, whch scaled a continuous xray or white xray” The continuous ay ste energy emitted a an xray when the elacton cient ona specimen is bent on ts waecory and decelerated by the electrostatic field of nucleus. Thi xray doesnot have a value unique tan element Therefore, the xray intensity ater exclu thie background is employed for quanitatve analysis (6-12. (Characteristic xray Continue x09 Fig. Xray Specrum of Stainless See! Specimen with Energy depecive X-ay Spectrometer 4) What fs the extent of the area (spread, depth) In which charactertstc x-rays are produced? ay analysis wih @ SEM is 2 mice-are anys or colecting the nformaton na microscopic ray generation area, sts very important to krow te rea (Sead, depth). ican be though that ‘he ay goneraton aes les down oa lvel at which he ncientlecton anergy reaches the rial ‘exctaton energy capabe of excing me characenstc xray pnmanly excited ay generation area) ‘as shown in Fig. 4 Therefore, the generation area of Kine (ne) sealer than ha of in (A ne). This relationship can be modeled comparsively easly by Morte Ca snulaton. An ‘example of this simulation is shown in Fig. 5. However, his example is based on a infiesa ‘lecron beam diameter, Since a spread dv tothe elacron beam diameters superimposed actually, the cay generation aes may be larger than n Fig. 5. Furthermore, when to ormore elements coext the Muoresconceexctaton are, where a higher-enetgycharaterate xray exces the characterise ay of other elment willbe superimposed. For convenience, Table 1 las the xray ‘generat areas of repceserative elements at aceleratng volages of 25, 1S and SK It the ‘generation area (magneton) i changed by scanning he electron beam, ks XY plane is freely ‘enable, ut ts cep as shown Fig 4ration area jo mulielemen:apecmen) Fig. Kay Genereion Areain Element a api Me. ‘AL Si A ca ay cr Fe a Oe Mo Pa Sa a Ww PB Soecimen Incident elstron beam "bnergy: To ke¥ ‘Number of inedent Kline — Ltn (Kanda196) Fig.5 Example of Analysis Area Presumption for (Cu Speceen by Ment Calo Simulation “Table + Approximate X-ray Generation Area in Nain Eleni susie | Density uate | (elem) a 270 235 207 155 rr 719 780 596 5.96 “eeleating vltage in| 599 768 490 678 ‘S01 282 156 1s 18 200 251 Line 7 490 3.68 689 335 278 151 126 20 Mine | ine 65 252 329 211 231 257 LOT 19k Line 329 2a 248 295 346 116 im bata OT ev [Mine | tne Line [ine5) What kind of x-ray detector is used in the SEM? For analyzing the elamenial compostion trough detection ofthe characterise xray (6-1)) generated by radiating the specimen surface wih an elecon beam, an Energy pareve Xay ‘Soectrometer (EDX or EDS) anda Wavelenath Dispersive Xray Specrometa’ WOK ar WDS) are fvalable. The forme is covfigred by a combination of Sold State Detector (SSDY6-6)) and ‘mul-channel pulse helght aaize (6-7), a the later by a combination of wavelength depersin ‘mochanism using 2 curved exystal and propotonal counter tbe (6-8), 6-9). Each ype of spectometer has advantageddrawbacks and are selecvey used according to aac purpose and ‘object A general purpose SEM equipped win EDXIWDX or EDXMWOX eystem equipped than ‘exclusive electron optics are oneal Leined EPMA (Elect Probe Mzo Arayee) OF MA (Oc Ray Mire Analyzer), 6) Principle and instrument configuration for EDX. ‘An ESD general used fr COX ea Si) detector wi Lit hae we ined w ype she crystal Sto neualze the acceptor (p type purty, Be), thereby foring an layer (in yer witout an electric charge as lustate in Fig. 6. When an rays incident on he layer, ‘lecron‘ole pars are produced in proportion te the xray energy and they are move othe respecive electrodes by he reverse bias ai, soa signal cent ows, The erergy for abaning a pair of electron and hols in aS) detection deve (whichis cal “ionization energy’) is about 3.8 V. Therelore, electron-hole pais are produced as given by diving te cide xray energy wih 39, anda pulse curentnavng a height corespending tote number of hose par i aken out ‘Ako since tho ayers oxen thickness of Several millimeter, characteristic xrays having a ‘wide energy range fom afew hundred eV toa few'ten keV canbe detected. The signal curentie _ampiied wth the prea, ts pulse waveform s shaped wih the proportional ampfer and sen to ‘tho mat chonnal pul tight analyzer (7). In vol operating stats, the O{L) detector and preamplifier are coped wit qua niragen player oxide) Hloyer _ nlayer oy alcrede | nts aver) 0m Ipaientexay Bs \ | / Fa. Operating Prince of S{L) Detects for EDX7) What is the multichannel pulse height analyzer? ‘Amulterannel pulse height anayze'6 used fr detecting the pulse heights ofa signal pulse curent ‘with the mul-channe! window and sor out the characerisic xay using the pulse heights as “dagrammed in Fig, 7. Th pulse height ofthe signal curents popodional to xray ney “Therefore, when one plots xray eneryon the abet, and the number of ays (ners) -cerrespaning tothe energy on the ona, 2 characterste xray specrum can be dawn. Elements ae qualtatvelyanayeabie by measurng the energy a the center ofeach peak nhs spectrum Window i Proprionl TORR , . = BS 7 * Output of E See at pee a SR Ee B Beer eo Channa wth 0 A0eVe) 9.7 Principle of Mutchanns! Pulse Height Analyzer '8) Principle and instrument configuration for WOX. WX is an instrument used fr sorting out and detocing only the aay ofa wavlengi that sais ‘ragg contion (vA = din, where , d and stand for wavelength, fraction gratngs ing neal and Bragg engl) using an analyzing crystal (atracton gating) The xray detection mechanism shown in Fig, Bs called a"WOX goniometer whieh selects the enery (or wavelenath, 61) ofthe cenaractenste xray aetctea by moving he analyzing crystal on We Wale a ay he ang 6 ‘The WOX goniometer is consgured so that he electron beam iadating postion ona scien, analyzing erstl and detector) tay say on a vidual cre called the “Rowand ice" even "whan the analyzing crystals moved. In practice, one analyzing esta cannot detect the ays win an elemental ange om Beto U, Therefore afew kinds a crystals fren in" are selctly used 96 requled. The WOX exclusive fr EPMA equipped wit plural goniometer having erent crystals o comprise multiple channels (usually 20 channels) node to minimize crystal exchange and hereby enhance anata tough. Used as an xray detect for WOK is 2 tandem type counter (69) configured by combining a gas flow type proportional count or low-energy tay detection and aga ils type proportional counte for high-energy xa detectionRowland cele (ama ele Sh = within 6,0 Brapg ange Fg.8 Pincple of WOX Goniometor 9) What the tandom ype proportona counter used in WOX? The atc ued WX tate ype Poor cor ened wig gb ed ‘pe peyote! caer hg array atau flow pe options out ere Xyddeconssintaadn Fy 90a na wastage leney one teed A lw 7 ean use Ug a pose ted epee pean nea vacum) thre contr anes hme Pg Eepotona cer e, reed gn 860% Ch) anys owe nan, art econ priced mb pece aatn clea ne Pegu eectode to cbain a Gas ow 2 BAO IO ed type Soetcome oO ae the other hand, 3 —_ narerwgyeroy Lanse pesen gh he Ba famatbe ne! katona ncn tho Xa recent ine net ype provocateur, Bi they cg sora oretn te 1 sare way sae gt Tigh ne tow pe Arion Xe ion 2 Electron Wigheenerey ry | Toanalyzer +—4 jt Fig. Structure of Tandem Type Poporionl Counter Empoyed for WOX o10) Are there any particular cautions to be observed In analysis using WOX? WOX has a goniometer (6) vertcaly mounted (vertical ype) or horizontally mounted (nrzonta ype). For using avers! ype WDX itis necessary to algn the posfon (eight) of specimen surface with he focus of golomeer within an accuracy range ofa few um as shown in Fig. 8. This requires thatthe specimen surtace be mior-fnished oa fa plane within an eor of few um (7-5) and thatthe Z-rectonalpositonng(helght austen) cf specimen be cared out sc with he ‘optcel mcroscope. However, a haizonil goniometer does rot need such stk specmen postoning and can be handled n almost he sare way a¢ an EDX. 44) Waat are the differance hetwean EDX and WOX? “Tablets he diferencestetween EDX and WOX. EDX fests hat detection senstvzy shih, ‘analysis is possible wi a smal pro current, mulpl elements canbe analyzed semttaneousl in ‘shor time, ete. On te ther hand, WOX features energy resolution a factor of x better than EDX, ‘elect iit high enough 0 detect vace amountiow concentration elements, etc. EDX is ‘mounted fo lnost all he SENS, and WDX are mounted to SEMs equipped wih a therionic-eision ‘election gun (1-2) and Schott elacton gun 1-2). “Table 2. Cherences in Characterises between EDX and WOK EDX mtd OX maha Shaakansoue alps of wa rial enaysie rt Siac ee tein Tie ehanoa ntanoe soniye pou msc Sete Slow (20 minstes or longer) Speemen damage | Slight Heavy Mounting space | Snall Large 412) How is quantitative analysis performed? "tis tfc determine th concentration (xefelement Ain an unknown specimen ‘imply om the rao of ay intensity In to the xy nen as f standard specimen (100% concentration), arly ludlag. The reason for is shat the folowing ZAF elects need tobe taken into account <> effect meanng thatthe coourence of character xrays varies with tne mean atomic umber (2) ofa specmen, <2>°A fect le, 3 Fig. 10. ZAF Etec in Xay Emission om Specimencharactors xray goneratod in specimen receives a sf. absorption by he spacmen unt t ‘escapes into vacuum and <3> "Feet, Le. cen characters xray subjected to orescence ‘exetton by othr xy (866 Fi. 1). “Therefore, the cencenationC, in element Ain an unknown specimen is ttainableby the folowing ‘equaton taking each cerecton ofthe Z, And F effects nto account. Casals ZAF ‘An actual ZAFcorestng cleltion woulé become sinficanty complete fra mutipe-lement specimen. So, conputris generally used fr this calculation. program fr this calculation i Incorporated nal ED} and WOX systems. Therefore, analysts do not peor the ZAF correcting calculation drecty by hemselves. Rather, tan be thought that C, acourcy is dependent substantaly onthe measurement accuracy of fas Inthe folowing secton"7, key pots for Improving this measurement accuracy are covered. Alo, the standarcest quantitative ana, wien a quantatve aralyss scared out by using a database on the xy tenis of standard spsomane inetoad afaing 2 eandardepecien, has been put ino praia use inthe marty of Instruments in this anayical category and effectively utiized for determining approximate concentrations, 7. How to improve accuracy in x-ray analysis. 41) What should be observed in order to improve the accuracy in x1ay analysis? For carrying out xray araysis wih anigh accuracy, te folowing requirements needio be met <> licent emision of the desired characteris: xray, <2> excision ofthe xrays generale in other ‘nan specimen (or trget keaton) ftom detection, <> resticton of xray generation area (ts spread, dept) wiin the desed naysis area spreadephn), minimization of ey generation sea, <5 ‘fatering of specimen surace as far as possible, <6> absence of pseudo poaks in EDX ele. Some ‘of hese -equrements do rot age with each ther, bl appropriate condions shoul be emplayed in response o een anaes purpose 2) How ean characteristic xrays be efficiently produced? “The rat of characters x0 tot luo backround (etnvous ay 6.) lon os has relationship withthe rat of incident electon energy Eyto eta exciton energy (6-4) Ea 38 shown in Fig. 1. Asis event fom his ‘ue itisefoctve to select an EE va within 2103 forthe mosteffient ‘generaton ofa characterise xay. ‘Attouphsatsng his canton ‘iutareousy for mull characteristic ‘ays fleutn actualy, ti import to select an acelrting vtage at which athe characters rays tobe dotctod can be excted ad he characterise xray cof parila terest canbe exctod most ficety among al the ays Fig. 1 Relatonsip between Characteristic Xa tens sandiego lecron Enero (Aceeratn Votace)'3) What should be done in order to avold detecting x-rays produced from other than the sample (location of interest)? When the detector and colimatr ok rightino the electron bear iraaon point onthe specimen surface as shown in 2), the ays produced tom otter than the specmenare not detected usually, However, wen te detector and collimator lok at part af he specimen ole because the specimen poston ls devised as shown in 2), the xy excted bya catered electon onthe surface of he special tected. A wen Be spocinen poston fuer deviated and the detectorcolimato: loots at the specimen chamber wal a shown n Fig. 26, the xrays produced rom the specimen surface wil hardly be detected and the ays exctod onthe specimen chamber wal wil ‘mostly be detected. Therefore, analysis is always required inthe status stown n 23), but the condition in Fig. 2.) 0°) may be aranged unconscious, because a SEMspecimen has a complicated shape, So aterton shoul be pa Eomeet 9 |(iaaa 9 “ ‘Sink wal Sentered Li “4 Reber mall Fig.2._Undesrabl Detection ofXsays Prodvee fom Other Than Specimen (ocaton af intres) 2) Corea specimen poston where detectrcalimatoreoksritint specimen )_Detectreatimator leaking at specimen holder due to devon of specimen positon ©) Detectorolimator coking at specimen chamber wall due to fare dewation of specimen postion 4) Ie thera a mathod for raducing the x-ray ganeration area? For reducing xray ganeration area €-4) na bulk specimen the accelerating volage neods tobe lowered. However th characteristic ays which can be exited are ited at alow accelerating votage, so the Land Wines (62) wl be detected main In some cases, the Land Mine peaks ‘may overiap onthe peaks of cher characterste xray In such cases, high accurscy analysis can be blaned by WOX ‘Als, afl inthe accelerating vltape increases the electron beam diameter of SEM (2), which ‘may broaden the xray generation area. Actually, tis necessary to optimize the condense lens and objective ens aperture so that a necessarysuticient ay signal btsnable andthe electron bear ameter canbe minimized. However, pariulat for miro-are analysis itis eflecve to use a SEM ‘aulpped with 2 Schotkeyelacton gun (1-3), 1-)) by which a comparatively smal electron beam Gameteris bianabe even ata large probe curent, n'5) How does the shape ofthe sample afect the analytical accuracy? men the specimen surfaces extremely uneven, anayical accuracy would be degraded because <> advance of xrays to he detectors blocked, <2> a calculation emer curs due to change in the ZAFefocs (6-12) and cher. Therefore, ts deemed desrabie to Raton th specimen surface a8, far as posse by mechanical posing after resin embedding, ec. as shown in Fg. 3. if fateing process is unusable for some reason specimen iting nd oation need to be adjusted so hat vance of ys toward he detector wil not be blocked andthe ay take-off angie wilt chang. ‘Als, ifuence by the intral structure of @specmen cant be neglected 8 stated i Fig. 4 Figure 40) shows thatthe elemental are of interests strbute inthe form of hin fim sie @ ‘specimen, Inthis case afl nthe characterise xray intensity ofthe target elomont cannot be Genie. Figu )s an example showing thatthe ditbuton ofthe target elements narow onthe ‘surface, but wie and deep atte inside. In this case, the characters xrays reproduced fom a far wider are han that ofa secondary electron Image. Figure.) lusratos a case where a target Ton which i nt contained in the matrix detected ‘Thus, a wrong analytical resut may be obtained depending on he shape of «specimen, but ts fective fr ensuring accuracy to measure as many analysis points as posse and obtain an average vale. Since EDX and WOK analyses ae basally ‘micro-area analyses, a mean value among 2 umber of measurement rests shouldbe cbinined Fn 5 camp of ay Anais {er determining the macroscopic compositions! eeerean, remade ek ary infrmaten of specimen, * ru Le] al lec on beam » Fig. 4 Roltenchip between Diferent internal Specimen Stuctres and X-ay Generation Aros 216), What kind of poeudo (Artifact) peaks appear in EDK? Main poeudo (aie) peat in EDX analysis are described below. > Escape Peak son incidence of characteristic xtay on S sol state detector (6-6), the SHK nes excod ‘As aresut some energy af he Inedent characte ay & lost, wich gives isto peoudo peak (led an escape peak), Therefore, he escape eens cee smacr groan Seertveo aren Sra dence aes laren) aa secre eae... eens rtecnte rs angen inant Sore > mre ‘when wo chaactenste >erays ate inedent onthe “detector in shorter than ts resohing tie, the charges cue ‘one respective cays canrot be separated inthe detector. “Thertore, a pseudo peak appears at a postion ‘comespondng tothe aed ‘energies. This pakis cle ‘sum peak. Figure shove an anaiyteal example of a SO; Specimen. Tho upper Fig. 6 Example of Sum Peaks in Analysis of SIO, Specen spectrum ina) represents a case “where a large number of charactrsc xrays are incident onthe detector because the probe curent ie exceesva large. Inthiscase, sum peaks ae vale athe postions corespancng tthe ‘enoiies of O-Xiine © SHK ne, and Si-Kline + S:K nes. nuh aconaton, the ploup rejection functon ofthe proportional apie is rquenty activated, so dead te sreased 10 35%, For preventing oocurence of eum peaks, is necessary to edie the amu of incident x-ay per nt time, for which eduoton ofthe probe curent i etlacve, The lower specrum inb) ste one measured wth the probe curenteduced o about 1/5, Inthe eat, the eum peaks dssppeares and the dead te was ehortenes to 18% n<> System Peaks During xray analy, backscateredelactons and xrays are ting about near @ SEM specimen, and unnecessary xrays fom ob than th element contained inthe sample are generates cverywheroin the specimen chanber. If the detector looks at an unnecessary xray generating location det, the xray rom wl be detected asa system peak only to downgrade the anaiytcal accuracy. Before star of your analysis, thereto, itis necessary to chock fr sytam poaks by using “a carbon (6) specimen which des not contain impurites. As aprevenve measure, tis essential “tat the cotctr looks sight in the electron Beam sadiating postion ona specimen as explained in7-)._ the sytem peaks sillappear, the specimen shape, structural matenas nea the specimen, _climator postion of the detector et. should be reviewed 7). What should be done to achieve high-accuracy EDX analysis wits Une low wacuurn SEM? For EDX analysis of @nonconductve specimen, itis commen to apply thin coating fmt the ‘specimen suaco._In this regar, imaging in alow vacuum of afew tn Paor more is advantageous because EDX anaiyels canbe cared out without specimen coathg. However, characteris xrays might be generated i substantaly wide area because the ident and backscattered eloctons are ‘Scattered due to colision wi residual gas molecules in alow vacuum envonmert (5-4) 'As is wall kooun,eacton scattering va low vacuum envrenmentineeases suddenly when ‘pressueexcneds 100 Pa and de oth phenomenon, the xray generaton area widens suddenly ‘2 te inensty of low-energy ay fas duo to absorption by the residual gas molecules Hence, 2 pressure range fom about 30 Pa where a charge-up phenomenon canbe reduced Yo 80 Pa where eecton scattering and xray absorption ar comparavely smal sconsered an ‘2epropriate EDX analysis conden wih alow vacuum SEM. Figue 7 ghes an anaiytca examele of ‘he sutace ofa heat resistant sheet fo eat sinks at accelerating vokage 15 KV and pressure 20 Ps DDotecton of unnecessary element peaks de to seaterng was at a negligible lve, and loweneray ‘elements wore detected wth ahgh SINrato, Fg. 7 Analytical Example ofthe Suriee of Heat Resistant Shoot Aenalaating wotags 15 V,gperiman chamber pnesita 20 Pa "8. Principle and application of STEM 41) What kindof instrument isthe STEM? ‘ASTEM (Scanning “Tanemseen Electron Mroscope) isan instrument ‘signe to ottan a magiied image twoughdetecton of the lwansmites an scatired ‘lactone (9.2) by inating 2 thin-simspecinen (of about 100 im tek) wih a convergent ‘lecton beamvileseaning t ‘two-dimensional on XY plane 28 senemately lagramed in Fg 1. Thetnsmited lectons cary information about the donsty and crystaine state ‘ofa specmen, while the Fg. 1 Instrumental Confguratonof STEM catered olooron provide Information about compositional astrbton. ‘STEM are oughly cls fabe ito 3 ypes:<1> @ TEM to which electon beam sesningfuncton ‘and detector se acded,<2> an excuse STEM instument equipped with an elcron gun fo 200 KV ‘or higher and <3> a low acceleraton STEM (up to 30 KV) wih a STEM detector mounted tothe SEM column, Expbined here's the characterises and operation metod ofthe low acoaleraton STEM based on SEN. “The low aczleration STEM uses the same electron optics as SEM forts mechanism for ‘nating a sgecen wth a convergent electron beam, to which a specimen holder for mounting thi-fimepecinen Ske the one fr TEM, a bigh-elé detector or detection of ansmited elecons, 2 atk ol detetor for detection of scared eecros, ete are added. Employed as thse detectors ‘163 combinaon of sentiator and photomutiper, asl tate detecter, mechanism fr detection through conveting the ransmitedscatteed electrons nto the secondary electrons, et. Wita ‘TEMbased STEM and an excusve STEM which use high accelerating votage (generally 200 KV or higher, stomiclevel contrasts obtanablein the same way a6 TEM. By contrast, wit alow ‘seceleraton STEM, arestictons imposed due to alonger electron wavelengtn. However, alow ‘ccelaratngvalage, sharp contrasts oblainabe because eectonscattoring is age (scatering ‘owe high)even fom a low-density specmen. Therefore, appcaton of alow aceleration STEM is expected ian extensive fed covering polymer materia, semiconductor mater, nanotechnooccl mater, 82) What are the charactorstics of the STEM signal? ‘when he electron bear is projected onto 8 ‘hrm specimen, the electrons subjects to ‘asic and incase scatterings (3:2) and hese transmitted though te specenen witht being ‘scared bot come outin the indent beam ‘vancing cect ae shown in Fig. 2. Now t's detect ony the transmit electrons by shutng ff the satered electrons wih the bright aks ‘aperure. Now, he specimen aea having high donsy is observable 35a dark area, an that hang alow density a6 a bight area co far 3s specimen hckness 8 even, Such an mage is cal a "brightfetd STEM image" Conrast of this mage becomes higher a the acoalersting votage is nereased futher Algo, case of Fig.2. EtcronTranamision and cxysaine specimen, theconrast which reflects he __Sttterng when Electron Beam Passes condtin of electron cifracton is euperimpased, 20 ‘ough Thins Specrnen the area saisyig tis conation i payed in dark contrast. (nthe ther hand, an image fermed through detection of scattered electron wth he ark fk detector scaled a"drk-feld STEM image” Because the scatenng ange of seated elecvon fers largely depending on specimen thickness, density and mean atomic number, the dekfls elector needs io be mounted at the optimum postion fr each specimen, Usual the shape and mourtng poston ofthis detector are optimized 0 thatthe detectors ‘pplcabl to specimens in he widest range possible. Sore models of STEMS are equipped wih 2 ‘mechanism for changing the detector poston fom outise vacuum, ‘A present, he escape angle of scattred electrons fom a specmen can be estimated by smulaon This feature makes the use of low scoelerationder feta ‘STEM images easier. Figure j= aa shows an exampie wih 2 Se ‘specimen thickness of 100m, From tis Fou, tis understandable that nthe Setrbuton of catered ‘ection angles, the maximum vale reached at higher angle ashe specimen denety rises. Acorelsion noteable between the Fig.3. Example of Morte Caro Simulation to Determine gle specimen deny ana the Distribution of Seatered Electrons with 10 Kinds of Thin numberof eateed lactone ‘Specimens (100m tick) %win an angie rane rom 400 to 800 mrad enclosed by red box in Fig, 3. This correlation ‘graphed in Fig 4. From tis fg, ti confmable that te number of scattered electrons increases almost linear for sen the specimen deny. Hence the mage contrast hich rete the specimen density (or mean atomic numb) ‘btanabeby detecting the satored electrons wai a range rom 400 9 800 ma, so the compositor sstbuton of specimen can be krown bya darkfld STEM image. On the other ‘han, wnen he satered electrons Blow 400 maar decid, the contrast which refets the capability of analyzing very narow area thanks toa smal lacon cating dameterin specimens (8-2), 2>Z correction alone being sufi, Le. no need forthe ZAF corecing calculation (6-13) unikeanaiyss of buk specimens and <3 high SIN rato because lass atc by continuous xray (6-3). Since thethinfim quanttave analyls sofware is icorpratd inthe major of EDX analy systems, quantative values ae readily avaistie, However, one should be cael about the analjas because system peaks (7-5) may be caused bythe characterise x-ays fom a specimen supporing gi, Figue 6 compares the xay mappicg images ofthe cross sectona structure of a mulbiayer _pscimen inccing Al and Cr layers which was formed into buk or hin fim. Wn the Bue ‘specimen, layer stuctur can har be cone, bu the Altayer (about 180 nm hick) and Cr layer (about 100 rm Bick) ae leary ise withthe fim specimen. Thus, insiming of specimen can enhance the resolution element mapping inages remarkably 9.6 Comarson of SIWAICISN Muttlaver Cross Secton lmanina beiween Buk and ThaFllm Specimens ‘Specimen preparation: Cross-ectining and thin ng wah FI, ‘Accelerating votage: 15k, Instrument used: Model S-4700 FE-SEM 4) What isthe method of preparing samples for STEM observationlanalysis? “The methods for STEM specimen preparation are almost he same as for TEM. Dispersion method, ‘miertey, FB ili, we ety weed They ae wlecvly une i espurse tthe object ‘and purpose of cbservatonlanalsis. 1) Dispersion Method ‘Such fe powcsery specimens (various nanotechologca specimens, ec) through which an ‘leon beam can pass eal ae usualy espersed on a grater pacing carbon supporting fim ‘ont Inconeete procedure, such a prwcery specimen scspersd ina cspersion medium prepare a suspension, whichis rppedon the carton supporting fin fosowed by dying 2 strated In Fig. 7. Asadspesion mosiun, wae, rehanol, butanol mylene rte kes wed. Because @ ‘mediums reactivity and persion elect dfer rom one specimen te ancther, some tal and oor wil be equred. 1's also employed to par he specen crecty onthe carbon supporting fim without Using @ dspersion agent ans hen give vations o ight spay ai oder to Bow of excess specimen. A grid with carbon supporting fm is commeriaty avaiblei Diggertion or pin pocimen stv minutes eapeSn ‘carbon VA el «tie Gemaete fe Fig. 7 Preparation of Spacnn for STFU Chsarvatn/Analyss by isparlon Mth 2) Merotony “This matted has long bean used fr preparation ofbologcal and polymer specimen, and receniy ppl alec to hin ming of metals and semiconductor materi wit damong knife. Thecuting pencil ofa mcttomes as shown in Fig. 8, ea specimen cut by moving I verily wth respectto te edgect a dlemond knife, Because he veical mations of specimen and specimen feeding motons are al automated, a numberof hinfim specimens can Be prepared aie in succession. In case ofa specimen consisting of materials dierent in physical characteristics (nardness te) such asthe specimen AB in Fig. 8, there & drawoack tht peeingis apt to occur at the boundary ofmatarale Aand 8. ut this rawbac canbe improved, fr example, by rein lembedeng fer sandwcting such a specimen wih dummy materais. For deta c the proving meted, rer othe erence document athe end fs text Fig.8 Appearance of Mirolome and is Cuting Prince3) FIBNethod ‘Te FB (Focused Ion Beam) method is 2 hrm preparation method under rapid dissemination land festures hata spectic area alone in a specmen can be formed int thin fim using focused alum (Ga) ion beam. The base 3 unctons of FIB are shown In Fi. 9. Athin-fim specimen ts Prepared by usng allthe basic functions. Fs, a SIM (Scanning on Mleroscope) mages formed ‘trough detection ofthe secondary electrons ejected upon radiation af the lon bear, and while ‘observing this mage, a specimen processing postions Getermined. Next, a desred part the specimen is ct cut bythe soutterin con. and than he cau specimen tis dante on the specmen nee bythe depostion function, The whoo process o this specimen preparation e ‘aries outwit micro-sampling unt mounted tothe FIB system. An example of ewing the detais ofthis process wth SIM images is inzeauced a Fig 10 Lets begin wih dterninaton of the processing poston wih a SIM Image and depos tungsten |W fim or proketon as shown in Fig. 10.8). Then, retict the spacmen are of intrest to a small ice of about “5 um wide by means of on beam so tha the ema pece ie supported at oly he lccation (micro-nidge) indicate bythe arrow in Fig, 10-8) Titthe specimen and cut of bottom by ‘he on bear (58), ae then bond a probe tothe smal piace by W deposi (e004). Next cut of the mcro-brige as shown in Fe) and tke cu the smal specimen piace comely fom the oviginal specimen. Subsequent, sck te small specimen piece tote specimen holser by W

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