Table of Contents Chapter 1. What isthe SEM? 111 What can we do with a SEM? 1 1.2 Principle and Structure of the SEM. 1.3. Procedure for SEM Observation Chapter 2. Sampling 21 Toole Used 22 Sampling 29 Metal Coating cies teeeeeseeees 24 Ion Miling Chapter 3. Lets Observe the Following with « SEM! 3.1 Machined Products, Materials 82 Semiconductor Wafer, Liquid Crystal Display 33 Biological Samples eee 34 Foodetuts Chapter 4. What causes these images? CChaptor 5. SEM Instruments Available Chapter 6. Q8A for persons wanting to know more about the SEM! 6.1 Concerning formation ofthe electron beam «s+eseesseeee 62 Concerning Evacuation 63 Generation, detection and usage of SEM signale 64 Viewing conditions for acquiring good SEM images « 65. Principle and applications of low vacuum SEM 85 Generation/detection of x-rays end elemental analyse method 6.7 How to improve accuracy in x-ray analysie 68 Principle and application of STEM ses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 ‘observe objects smaller than this, an optical microscope or electron microscope must be used. Na rus Lactobaclus Ha Water iea Honeybee 20m 000m ‘im 10em {00h T4rm TO stm 100; Ym 10mm 100% Electron microscopes are available in a scanning electron version (SEM)" and a 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 ofa specimen at high magnification, We will introduce tere the features of the SEM, “FT SEN Siang Heaven Maoaseo= Features of the SEM 4. All solid surfaces can be observed in a range from low to high magnifications, 2. Focal depth is greater than that of an optical microscope, allowing us to acquire a stereoscopic image. 3 Combination with an x-ray analyzer permits compositional analysis of a microscopic areaNow let's compare the images obtained with an optical microscope and tre SEM, ple used is a fiber employed in parasols for blocking ultraviolet rays. ‘Observation with optical microscope Fiber observed with an optical ‘microscope. Although he OM provides color informaton, thas a shallow depth of focus, and when focusing onthe cic pat in the Image at the left. the partion having a slight ferent height ‘comes out ae an unclear image, 110 magnification “The sample was obsersed with an SEM atthe same magnification as Used withthe OM. Altrough the SEM image is black & white (lacks color information, it has greater ‘depth of focus and provides stereoscopic informaticn, % 140 magnifieation % 4,000 mag, % 15,000 mag, |When observing an SEM image with the magnification increased to »,000, inorganic ‘matter (whit patcies) that are used to block UV rays can be eeen cispersedin the fiber. Note that SEM images include secondary electron and backscattered electron information (explained late), andthe above are secondary electon images, By futher increasing magnification to 16,000, ican be eaen that the inorganic matter becomes paticles of 100 to 500 nm in size. A cross-sectional observation can be mads next to S2e how the inorganic particles are dispersed inthe fiber.Observation and Compositional Analysis of Fiber Cross-section Backscattered electron image (5,000 magnification) ‘The cross-sectional structure of the fiber was observed witha backscattered electron detector. 3 ‘This permits conformation of how the white partes are dspersed in the fiber. Let's put this to (compositional) analysis, (Xray spectrum of area TBE X-ray mapping enclosed in rectangle above image of ¢ and 7 First ofall e's cu the fiber observed before and observe its cross-sectional structure via a backscattered electron detector. Since a BSE image permits Selecting a ference in average atomic number asa dference in contrast, 2 location having diferent compositional elements can be clearly seen. The white listening particles are inorganic matter, and one can see how they are dispersed inthe fber. Also, when an electron beam is applied to the sample, characteristic xcraye vil be produced as wel. By attaching to the electron mierosecpe an xray ‘analyzer that captures these xrays, tan be seen what eloments exist and vier they are locate. By conducting xray analysis on the part enclosed inthe rectangle on the BSE Image, ts seen fom the spectrum that tanium (i exists inthe sample. Now, by conducting xray mapping on carbon (C) and Tiin the same visual eld as on the BSE image it wil be clear that te fiber contains organic mater (C main) ‘and that particles of (actually TiO) which serve to Block UV rays are dispersed int,1.2 Principle and Structure of the SEM Lets leam the principle and structure ofthe SEM.- What is the SEM? “The SEM is an inetrument that scans a sample surface wth a finely converged electron ‘beam in a vacuum, detects the information (signals) produced a that ime from the ‘sample, and presents an enlarged image of te sample surface onthe menitor screen Incident electron beam Backscattered electrons —7 (BSE image) Cathodic light — (CLimage) ~_ ‘Secondary as electrons: (SE image) ‘Sample current XK Signals produced from sample 7, (Sepa podicad tom sar By iraciaing the sample wih an electron beam in a vacuum, secondary electrons, backscaterad electrons, characteristic rays and oer signals are generated as ingicatedin te figure above. The SEM mainly ullzes secondary electron or backscatlered eleczon 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 structure ofthe sample, ‘Backscattered electrons are those reflected upon striking the atoms composing ‘the sample, and the number ofthese electrons is dependent on the ccmpositon (average atomic number, crystal orentation, ec) ofthe sample. A BSE image ‘therefore reflects the compositional distbution onthe sample surface. Besides, an xcray detector can be mounted to the SEM for conducting elemental aralysis. So ‘the SEM is usable not only for observing the sample structure, its also applicable ‘a8 an xray analyzer for determining what elements are included inthe sample and {o what degree.Configuration of SEM cea jeaac) = Geese) (5 Secondary oleton detec] "Vo v[As shown inthe gure atthe let the SEM consis maint of column, specimen ‘chamber, display and operating section. The interior ofthe column is Kept ina high ‘Vacuum and the alacvon beam produced by he electron gun (pir testking the ‘sample) ie converged into a fine beam via te electromagnetic lansee (condenser and ‘bjeeive lenses) And by applying a scan signal tothe dellecton cals, the electron bear is scanned along the sample surface. The specimen chamber fs equiped with @ ‘specimen stage having a specimen goniometer, a secondary electron detec or detecting signals produced fom the sample, and depending onthe instrument, backscattered electron detector and/or an xray detcter. Connected below the ‘specimen chamber fsa vacuum pump fo Keeping the Ineo of he column and ‘Specimen chamber Ina high vacuum ’A mechan at emis electons rom a metal and accelerate thm ina stor eectic fed There are the types of electron gun according to the method of missin — fd emission ype (FE) election gun, Schotxy elecron gun and thermal electon gun. For dette rfer to Chapter 6 2, Condenser ons Tir electromagnet ens (col) used to converge the electron beam emda he ‘locron gun io fps bean 5. Deflection cot “A mechanism used to sean the electon beam in X andY iesons and change the area (reagneaton tobe scanned. The SEM magnifica, 38 seats inthe gre, {otrminod by th rato of wih of mage deploy ooa (Lo wi felon teem aoan on the sample, 4. Objective tone ‘Used wo converge the electron beam int fe beam and focus tonto the spe surface ‘There ae thee types of ens, inlens, series and outlens, according oe object of ‘observaton or resolution. Refer fo Chap 6 for etal. 5: Secondary election detector fic captures, converts to elect signal and amplifies the secondary eetrons produced fom the sample. Refer to Chapor forthe metid of aetacton 6. Display ‘Converts the detects and amplified secondary electon sina to bghiness and proves fan eniarged image 7. Vacuum pump Evacuate the clan and spacmen chamber toa high vacuutn eval (104 to 10° Pa). efor 'e Chaper fo datas on evacuation,1.3 Procedure for SEM Observation We introduce here the procedure for SEM observation using the S-3400 SEM as, ‘an example. (1) Startup of instrument | (1), Tum ON power ne nstument (2) Log nto PC and then startup the SEM software (2) Preparation of sample to be observed (©) Atachconduetve tape specien stub and then mount he sample on his, (EQ Sarple (Refer to Chaptor 2 or detailed contin ge cee oeeet By wre (4) Set specimen eb on exclusive holser and aut height wih "eight gauge” (Refer to instruction manval of applica ume) (3) Setting of samole to microscope: (6) Press AIR on front panel of column and inreduce air into specimen carber. {@)Pul eat specinen stage yenly an se peciten hater on cone’ osiage (7) Press EVAC on rot panel of column and evacuate specimen chamber. (6) When evacuaton of specimen chambers fished, start observation of sale | (8) Click the accelerating voltage ‘ON icon. (ovata inne ape ASC os ges srl Ara el (12a er tte arated ett eg een (5) Acauisition and saving of imeee (12904 Seon ct ste ard ee tl (1) aa scapnrn box age et kon {1 saeaatoeernptate ane ace "Baw bn wa EVAO/AIR switch mentioned in steps (8)(1) at loftChapter 2. Sampling Introduced here isthe general method of sample preparation (sampling) eZ em, =e 2.2 Sampling (1) Bulk sample, fm, te. (2) Powdery samySpecimen | uss "Seoncn sue se a nat be Poe ens drnn va Exide) Snir athe encores sea paste SGOT Raussen te Seguersaeenar woeser | Unter snatch Blower Been | traanigots tre rts gmeata see cn (Fe ffs, samples ontaning a ‘revraon eat a te ee ‘setantaus Seta (er epson te) “ig eee an ‘nciospr meses Peart2.3 Metal Coating (1) Purposes of coating ‘To make the sample surface conductive (prevention of charge-up) “ Toincrease the producton rte of secondary elcrens (nerease Image inormaton) * To prevent damage o sample (2) Fim thekness of costing 'Athough a hicks cf several nanometers standard forthe fm coating, vari with ‘he magnifcaton used forthe cbservaton. A somewhat nner coating fs tae fr hgt-magnfeaton abesraton And for observation at ow magrifeation, sgh ticker coating wil provide a clear mage having a good SI rato, (2) Kins of metal targets ar | Sou For ‘Evaporation fin suitable fr ‘generalise ‘SEM cbservation: ‘Aveo | Gotdpatacium | “Sekt | Coating paricies | 1 Fi of uniform quaity having epg | Patan 1 | adequately ne partles pall ForFe- | Fine | 2 Secondary electron Se Gacharge rates good. et | Patina 23. Sable against ton “Te particles ofthe coating fim become fin the der init inthe above table. On a ‘sample coatod wih 90, the parcles canbe obsorved at a mapnifeaon of £0,000 ot ‘60,000 and ihe. Fr this eason a gold paladium coating ofen used wih a general. se SEM. In the case ofa SEN having a igh resol such asthe FE-SEM ae coating ‘im wih which tne partcles cannot be seen required. Therefore, since the pate stats ofthe coating fn varies wth the coating mai the target must be selected accordance ‘ite purpose. Aso, fr costng a same having an uneven surface, ts recommended © ‘Soni the contig tomes nie tng the samp mn arent rectons os chown nthe ‘ure been, # EE Shed Megnevonsputeng device cating of ale ving uneven uae (40 (carbon) coating ‘A vacuum evaporator is usualy employed fr carbon coating. Since the paces of the evaporation fm are fine and of ow dene, his ype of coating Ie euatl for ‘omental anayis or observation of BSE mages24 lon Milling (1) What son mang? on bear mling a tchnsque that izes 2 broad ion bear (BI) of aproxnataly 1 sm in dames discharged rom to gun spt alms fom the samp surtace, tis {bed for etminaing machining awe fem the sampe surface or preparhg rose sectional samples of multiple im ayes 2) Whats BIB on ating? 2-4 Surface processing at ming method) “The sample surface is unformly etched by trading the fon besm at anangle while rotating the sample ‘Main selestons Eiminaon of 08 fi or contamination rom a wide area of about Sam diameter on sample surface + Ezminaton of machining laws fom machined sample surface * Observation of stl pains cr layers formed by ral ming ‘nataton of BI at an ange ‘store (Outer view a IM-2000 on miling device 2.2 Grose section processing ‘An even cross sect covering a wide area about 1» 1 mm) ofa sample canbe repared ty placing shin plate on na sample and backing pat heen am radiated ont the sample, then etching around the edge of the shielding pte, ‘Main aplesions + Evalusionlobsenvaton of complex cracks or volts caused in machining a sample * Obsenvationlanatysis of aminated boundary + Cross-sectona observation of sample (papertiim, etc) suscep te stress 118 vertical ination aa y ‘Sample swing mt (er view of 3500 lon ming deviceChapter 3. Let’s Observe the Following with a SEM! 3-1 Machined Products, Materials (1) = = ‘Interior, cross-section sample >) Tage saris ([staing marr ebay monies a ‘cuting edge Sambo fact *ceenes tie beoned sere Example: Resin packing, Machined sample ‘BOA (Bal Ona Alay) ose secon tion‘Sarg gusgotbe Tad emuison "Roaursngatae 61 Checonmss wed {errnenm 3 ge ‘imose wh ih a negative voltage eel vote) sapped io he sae, an be econ bean ctelrndvi the soceon gov Solera pt ammo. Tac use of ames ames cosoaton {senses andlor i deagecbesvoton slow ean volage of 0 ora a oe ea wh “ERP lecwon Baascatring Pate ages ofthe cya ort san be sored {Gp Spt secon beam fackacatering dttacton an by atacing We yen (EBSD) ha Sloss ete SEM, fe ye onaraun of amet rr la song canbe red en peng3-1 Machined Products, Materials (2) = (Sampis of meen order Semper gap] ) ([Seeeewmmooaer roa srt owe foundation Fine metalic partes Cotas | Fea haw3:2 Semiconductor Wafer, Liquid Crystal Display ( Sues sbsonaion Cre econ aeenaton_] >) aa Tks on Sp We Sereno, Ss Ey POE 3 ee ; cote ete aee cao = t (Hetieat sca) — | aoe as aac acer = ' ears = | Fm pug cainquid eryetal ‘Opssnision of TFT (ine fm wansston) oe aoeton = rere pee | | (ereceee sting tae 2 ea ae es eo Tans peo ae {Geer tunis oe dion mye ot ern canara ows Shoo pokes be3-3 Biological Samples Underwater blotogeal mater‘Microorganisms (fungi) a [Sse sonn bon n-ne ‘acti age: Prtomoacaon a a Refer to preceding page 10 fr botgieal ample preteatment method,3-4, Foodstuffs Beamer Ea ton eee Foxcr a ssoums, | senane @| lat Setaortine | exo otaChapter 4. What causes these images? Probable cause © craeew © contamination Image moves 0e00 e ‘Sample structure cannot be discerned 600 Image is distorted 0C0e © cexin darnase Effect of external disturbance e Other “Causes and countermeasures are describes on te folowing pages. Image fluctuates: Brightness is unstable 0606 Cannot be focused ©0606@) wiraris the charze-un phenomenon? (Chargeup coors during cbeervation f on-canducive samples, and may be conspicuous {especialy when scan speeder magnieaton is changed, Gaow ae xamplesct the ‘chargeup phenomenon, cic |] Examples of Charge-up Phenomenon cape |] cen ' Ine elacton beam iradiaton are onthe sample surface, there are an incoming electron wp and an outgoing electron Now Io (0 = neg) 9 ated nthe above figures. When the sample surface is conduct, lols equal tp. But when te charge ‘becomes unbalanced, Ip does not equal, charge-sp wil appear and the suace potential ‘any Flowing are countermeasures forthe charge-p phenomenen, 4 Reaice the accelerating votoge, 2 Reduce the sample rating current 3. Apply mata cooing 4 eg eimape fom an aoe by stmincnng apes one 3 5. Observe images in ow vacuum mode. 6. Uilize alow-aocoeraton BSE sgn! liminte SE slgnal by means of ital Varying mechanism). Refer to 48 tyaugh 4-10 mn Chapter 6 for deal© rat is contamination? ‘The phenomenon by which gas molecules of harocabons exsting around the sample aloe on the sample de te etecron bear 'radiaton, then bond together and adhere to the sample surface is refered to 35: contaminaton (se Rgure athe righ). With the ‘econ beam iradatng he sample, te cay ofthe mage at at area decreases as shown Inthe fgue below let andi ecomes darker ——— ‘Te reason othe darkness i thought tobe cer thatthe mat ccumulted on he sample Surace suppresses the decharge of econdary ‘Seen rm he sample ‘sap of Sale Cotamintion “The following stops are required in order fo reduce tho contamination * Roducton of residual gas molecules in specenen chamber mprovemert of vacuurn eve) * Roducton of gas molecules derived fom sample ‘Concrete measures o achieve the above reductions areas flows “1 Use a miesnum amount of conducive past ote when mountng the sample in the 2. Thoroughly dry the conducive paste wth a dryer othe ke pert inserting sample nto the istument or obesvaton. 3. Heat and dogas he sample na vacuum device 4. Cary ct focusing ae quicsly a6 possible and avod observing the sare location for long ‘ime especial at igh magniieaton 65. Observe samples wie sagen he sample suroundings wih aco ap. ‘The reason why contamination is cenepcuous on he et site ofthe eecton beam scanning {x eat mei provided in lection Beam con ere electrons to rman te. To prevent a say magne fed om afectng te mage, a method e scanning thats “Synchronous withthe power frequency (50 cr 60 Ha) s uzed (power suply synchronous scan), ‘and requires a waiing tne before he sat of scan recent matod of preventing this Contamination fo eqp the SEM wth a boar Blanking function with which be electon beam aot iradate the sample uring he wang ime bear the stat of sean6 What is beam damage? ‘Tema change or chemical change occuring ona sample due to electron beam racatin is tpereate at beam damage, Teper ie ofthe sample due totbe decian beam 8 Aependent on 2 number of factors nclucng aceaertingvotage ae imensty a he beam, ‘observation area, observation tne, specie eal and heat conduct othe sare, and others Reha rel ard: Bllogseanece re array sacepe 0 hoa, anny ready damaged thetmaly bythe elocron coor. An example of thermal damege opoymerc ratrl onus oye eacon boas gen balw etna No been drape ‘Damage cso beam radeon Flowing are countermeasures avaiable for beam damage {Reduce he sample radsting cent 2 Lower the sceleratng vote. '3.Appy metal coating tothe sample (to improve heat conduct) {4 Observe he sample whe cooing © Effect of disturbance Fringe or istorson appearing ona SEM image profile maybe caused by vibration ora tray magnet eld. Countermeasures for mage dsurbance due to vraton are gen bekom. "Keep the nstument we away rom vibration souees suchas a-condone pumps 2 Do att high-otage cabs fom the coun come in contact wh the wal or ther ineaaten toms. 8. Donte the dat rom an al-coetioner out contact the column ret. ‘Countermeasures for'mage turbance de toa atray magnetic fd ate as flows 11 Keep the Instument wel away rom magnets eld sources such a Partormar or arge capacty power cables. 2. Shorten the working stance (6661-7 or 4S n Chapter 6) an apply song exctaton tothe ‘condense len 0 counter e eet ofa magnetic tad 3. Use a magnet fla cancel age afc vraton nape aleteby magneto aGore: 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 Image fluctuates | case of semi inlens SEM, + WD is long in low vacuum SEM observation mode. + Inadequate optical axis alignment + Objective aperture contaminated + Recheck the instrument parameters, Focus cannot be obtained 2%Chapter 5. SEM Instruments Available FE-SEM Lineup Ultrahigh-Resolution Field-Emission SEMs Inens type FE-SEM Semi in-lons type FE- ei : Seats eaten oe ae eee: ae Semi insens type Schottky Outotens type Schottky SEM ‘SEM (high vacuum) (lowihigh vacuum) lee | Senger, |Hi-SEM Lineup ‘Scanning Electron Microscopes | Out-ofons type SEM with thermionic gun (lowihigh vacuum) peace ae ierecces ‘Scanning Electron Microscope (Out ofens type SEM with thermionic gun (lowihigh vacuum) Agree hah aromas owen, {Spon oh nage set Dr (tees Pat wa on om 0 5 ‘Outofens type SEM with thermionic gun (lowihigh vacuum) “i a Tabletop Microscope eto | : A. Tabletop microscope (low vacuum)Chapter 6. Q&A for persons wanting to know more about the SEM! 4. Concerning formation of the electron beam 1) How sa tne electon beam formed? 2) How is finer election beam obtained? 3) What kinds of electron guns ae used inthe SEM? 44) What ae the difrences between the kinds of electron guns? 5) Whats the operating principle ofthe electron lens? 8) Whats ens aberration? 1) What kinds of objective lenses are used in the SEM? 2.Goncerning evacuation - 1) Why mustthe electron beam path be placed ina vacuum? 2), How is the evacuation performed? 5) What ments andor demented the vacuum pumps have? 44) What kind of maintonance do vacuum pumps requie? 3. Generation, detection and usage of SEM signals « 1) What happens when elections stke the sample? 2) How are backscattered electrons produced? 3) What kindof charactoristies do backscattered electrons possess? 4) How are backscattered electrons detected? 5) Whats he signal varying mechanic? 68) What ae backscatarad elacrons used for? 7) How are secondary electrons produced? 8) What kindof characteritics do secondary electrons poseass? 8) How are secondary electrons detected? 10) What are secondary lecrons used for? 4. Viewing conditions for acquiring good SEM images. ++» 4) Wat sa good SEM image? 2) nat effect does accelerating voltage or condenser lens curent have on inage quality? 3), How must accelerating votlage be selected according tothe sample? 4) Whats the function ofthe obyctve ens aperture? 5) How does working istance (WD) affect image qually? 8) Whats astigmatism and how is itcomected? 7) Whats focal depth? 8) Whats the charge-up phenomenon? 9) How is sample surface potential changed by charge-up? 10) How isthe image disturbed by charge-up? 11) Wirat are the advantages and disadvantages of sample coating? 12) Wnat sample coating methods are availabe and how do they differ? 18) Whats the principle of the magnetron sputerng methed and plasma fim foration method? ag‘5, Principle and applications of low vacuum SEM +++++++» 41) What kina of instruments the low vacuum SEM? 2) Why ist that an insulatng material can be observed without the charge-up phenomenon bby means ofthe low vacuum SEM? 83), How is SEM signal detecton performed inthe low vacuum SEM? '4) What are considered tobe the demas ofthe law vacuum SEM? 5) Please give concrete example of application ofthe low vacuum SEM, 60 6. Generation/detection of x-rays and elemental analysis method ~ 1) How are xrays produced? 2) What kinds of character xrays are there? 3) Are there any xrays other than the characterise ones produced by electon beam inaction? 4) What Is the extent of the area (depth, spread) in which characteristic xrays are produced? 5) Whatkind oferay detectors used in the SEM? '5)_The principle and instrument configuration for EDX. 7) Whats the mutichannel pulse height analyzer? 8) The Princile and instrument configuration for WOK. 9) Whats the tandem type proportional counter used in WDX? 10) Are ther any particular cautions to ba observed in analysis using WDX? +1) What are the diferences between EDX and WOX? 12) Mow i quantitative analysis performed? 7. How to improve accuracy in x-ray analys 4) What shouldbe observed in order to improve te accuracy in xay anasis? 2) How can characteristic ays be efficent produced? 3) What should be done in order to avoid detecting xrays produced fam othor than the ‘sample ocaton of interest)? 4) | tere a method for reducing the xy generation area? '5) How does tho shape ofthe sample affect the analytical accuracy? 8) Whatknd of pseudo peak appears In EDX? 7) What shouldbe done to achieve high-accuracy EDX analysis withthe lw vacuum SEM? £8, Principle and applications of STEM ~ 75 1) What kindof instrument isthe STEM? 2) What ar the characterises ofthe STEM signal? 3) What features are obiained by combining EDX analysis withthe STEM? '4) Whats the method of preparing samples for STEM observation/analysis? 5) What are the applications of STEM (EDX)? x01. Concerning formation of the electron beam 1) How i 8 fine electron beam formed? Inthe usual SEM instrument he econ L source (dameter fore bythe electron gun _Blctron (001-3 in chapter 8s reduced and made into fre electron beam (ameter ¢) bythe ‘condenser lens and abectve lens 2 indcated in Fig. 1. The condenser and objective lenses of ‘he SEM ae both slacromagnetc lenses (8). “The magnifeation Ms, Ma (or reducon rate in SEM) of thse lenses is expressed by M, = by, My= bf, and the fina beam ameter = 6 Mie -Athough would seem that could be made Init sate by reducing My and My, itis not quit that simple. Fist ofa bs shortened and My reduced excessively, the electrons Incident onthe objecve les willbe reduced and : = {probe curent (radiating cent requed for ‘Sample Astanas (WD) fomation ofan image wil ot be obained (see Fig. 1). Actially the condanserlens curentis Fi.” Scheme lerOttsirg a Fie Eecton Bar adjusted so that M, willbe minimized in the range here a suflcen probe curent can be obaines (4-2). Algo, since image distortion caused by lens stoeration wile aed (1-0, there sa nit the reduction Uy Mote opening angle ofthe elcron beam (1-5) Aperture Does not strike objective lene -Objective lene ‘Apesture 2) How can we obtain an even finer electron beam? In order to cian fine electron beam inthe SEM, the instument izes an electron gun fearing smal election source, a large cunt densty (current (Alem) per un area), and mal energy ath (energy vriaten (in eV) of ischarged elacvons, lus an objective lan having very ile oration. See) and (7-7) for more deta on the characteristics of he lactron gn and objective fons. Flowing ar points to keepin mind when sting the viewing condone 1) juste condenser ens current appropriately as mentioned on (1-1). 2) Use he objective len athe shortest possible wertng sistance WWD)(-7, 45) 5) Set an appropriate bore ckameterfrhe objet ens aperture i oder o minimize lens aberration 09) 4) Sine the emission current deereases with a lover accelerating voltage Ina SEM using thermionic source (1-3), ary out lament height austment ana bias adustment to obtain the died urent. 5) Be sur to cary cut astigmatism correction (4)3) What kinds of electron guns are used in the SEM? “Thermione ype gun ungsten han type, lanthanum hexaborite (Lab) fpe) ld emission (FE) ‘909 and Schoey type gun are general usedin the SEM. Flgue2iusates the configuration and prinple of electron emission foreach ype of gun. Electron emission is achieved inespectve cases by apphing ternal exctaton (applying energy to electrons while Nesting), by usinga tunneteffoct (forcing electrons ou ofan energy barr via a tong elect fel), and by using th Schottky efect, (lowering he energy barer by mesns of a stong elecic fl), wih which conducin electrons in ‘metal can overcome the energy bare existing at he boundary of metal and vacuun Carbon Heating power Theater PPI em Anoad 9) Themionizgun funasien hin vee) | | ®) LaBaun Tungsten i heated and energy ie Lanthanum hexaborid (26, having applied to conduction electrons in small wrk funtion lctons are ‘order to overcome the enerpy baer readly emits) is used instead of ‘st retavoowum boundary. tungsten — Heaeenoner SEES AL Bstraction rien ™ apne vant ale | ante Eten aston Staten in Etogcecrchidtcmneamion | | tercuin a2, sonst Sutectonpwrongecyatrd.” || tele’ anew ony Sade beurre necro ca Fig.2 Coniguration and Principe of Electron Emision wih Various SEM Elscron Guns 24) What are the differences between the kinds of electron guns? “Table compare the charactors of he tungsten hap ype thermionic gun, Lab therminle ‘4n, snd FE and Schotky electron guns. Important actors n the formation ofa fe electron beam ‘a electron source diameter, brighiness and energy with, and the FE gun excels inl of hese characteristics, ths indng wide use in high esokon SEMS, AS universal typeof cton gun, ‘he tungsten hap type therminic gun operates wih a relavely spe evacuation eystam and Provides a large probe curent, aris appicable oa wide ange of uses ran low vacuum SEM (5-1) Upto EPMA(G4). The Schotky guns sigh inferior othe FE gunn elcren sours ameter, brightness and energy wich whl xoviding a xge probe curent, and ie appicabe to 2 ‘mutunctonalhigh-esoluton SEM Festung high-resoluton observation plus xray ars uncon 66,68, ‘Table 1 Comparison of Characteristics f SEM Electron Guns lanham atin rngion | real ae ‘oui ca er aco Gatade work function @V) ee 107 10" 10 0 ‘Working a > eo fc 10 1 1 Cathode lifetime | ~B0 he Sooo | Tyear armors | ~Donthe5) What isthe configuration andior operating principle of the electron lens? leton lenses include magnet fl ons and electrostatic ns, andthe descriton here covers the magnetic eld lens tat is general employed in the SEM. The magnetic field ens serves to {focus the electron beam formed by the electron gun (1-3) it ae probe and iad tonto the sample surface, and the SEM utlzes one orto condaner leas and an objective ns fortis Purpose. The confguration and operating pnp ofthe condenser and cbecve lenses nthe SEM axe shown in Fig. 3 ‘The electron beam incent on these lenses affected by the magnetic fd prodcad trough the 9p (poeple) nthe magnetic pat, Is converged whe rotating around the opal, and forms reduced image of the beam onthe image plane. Note thatthe objective lens is designed so a not to Intertere wit sample movernent or secondary leeton, ay sepal detect (7,65) “This action fe expsined in furher detain Fg. 4. The lecrons emits tom each pont ofthe electron beam are focused ‘ont the corespending image ints by the election lens and form areduced image ofthe beam onthe image plane. The reduction rate Mat his tin ie expressed by M = bat). “The reduced image fom he ‘ake mp ae condenser ln becomes the ‘beam forthe objective fens, and the edad image fom the objective les is raced onto the sample. ‘Noe thatthe reduced mage Includes some cstorton caused byes aberration (1-6). The aperture angle ais determined geometrically fom aperture ameter ofthe lens (bore <éameter of aperture) and focal stance, and has a lage Infuence on tne characteristics ‘uch a ans aberration anc focal epth which willbe explained lator 44), Fig. Coniguration and Functon of Electon Lens Fig. 4 Reduction of Electron Beam by Mgnt Feld Lens o6) What is lone aberration? Lens aberrations minnie apherical aber, cat bean, diac and asigmatsm (4), among whichis Sito completly exch astomatm. ishereore recommended cary cut abseraton under conden nvAich thee aberatons ae miniizd n deo ban goos SEM rapes. 48) Spherical aberration a) Sphercal aberaton, a sown nF 68) ie a distortion cours by a tree In ‘convergent postions between electrons oman a7 ssing near the lors center an slacrons gassing at lecaton away om the center. ne exten thie tortion oie roportonal the cube a opening angle. Objeiv lee Gyisthe spheric aberatoncootcint and AERC the shorter be focal datane (1-5, te saiecthe Cy, Spherical bara can ‘thus be reduced by using a smait aperture bb) Doe data shot ncn. /} \ | Paensil rays Nowparasial Minimum bur cise inca ) Chromatic aberation Chromatic aberaten, a icicatedin Fig, bet enw 5, s caused by variation in energy (wavelength) of electrons incidont onthe lens, ad the extent of this lisorton det Objective lens spare econ hosing hh proportional te onory varaton SE end ee ee opening angle aC, isthe comatc ‘nergy See sberation coefiient and becomes smaller WC eAEE)a asthe focal distance becomes shod. ‘chromate aberaton can therefore be ° j reduced by decreasing the energy with ot ‘leeton beam (1-4), sing @ shorter fecal stance and reducing the opening angle =. Objective lez ‘Tne fect of chromate aberration f larger < 2 ne acceorating voltage becomes lower. «© Ditacton Difracon, as Mustatedn Fig. Se), is 2 tracton of electrons caused by resting the convergent angle (beam opening ‘ngie 0 electrons, anditcauses the Fig, Generaton of Lens Aberratons aud Their Extent beam towiden, The estent of his 2) Spherical aberaton, 6) Chai abersinc) Oacon sberation ds proportional tothe wavelength of eletons and in averse proportion fo opening angle «. Ahough can be reduced byincressing ie aperture dameter, te spherical and chromatic aborations ilinreas, So he aperture lamer must not be enlarge too much7) What kinds of objective lenses are used In the SEM? ‘Sphrical and chromatic aberrations of the obecve ln bacome eral by shatening he focal stance, Soin addion tothe out ens ‘ype ofabjecive lens generally used withthe a) letran beam ‘SEM, an indens type having a shor for highesoluion SEMS ac a srk 990 (or ae se nen type have been developed 8) OutotHens ype cbectve ens Wi is ns inetd in Fig. a), Secandary le vita ens is femed at a positon above the ae, lp ‘sample, so there ig a iit on how much ean be shortened, Ashough his makes trates unsuitable for high resolution SEM, is “= oe ee convenient for observation of large samples since a large working distance (WD; distance ‘fom lower face oflenspole-pece to sursce ot 4) on bytes aes tegen be ovied.Tha nin segndary BY depict fa ulivctonal SEM since E® “yoni porns ceareanrinay of magnate tater wth which akg magnet ld teva he sane in ra d ee] Inons type objective lens “Te feature of ths lens, as indicated in Fg 20) Ua been sted Semple Sonjctve tens because a samples placedin the gap between ane as upper and ower pole-piaces. Ils therfore applicable to ulatigh resoluton SEM, but © apc SeSSRUBEE Bhetton beam there ia tint on sample sz0 and itis unsuitable for obsening sonal magnet ‘atrial. Secondary electrons are spun ‘ward bythe strong magnetic fd ofthe fons ‘and detected by an SE detacor mounted stove the exting cll and es secndary Objective lene ) Snore earliniens) ype objecivetene electron deter) By ple pce Wh the snorke type lens, as indicated in Fig. = eo Virtual ens 63), a pole-plece gap i formed and by binging Sample the vitual ens close tothe sempl, ange ‘sarmles canbe observed ata short (> WD), Fig.6 Kinds of Objetve Lenses Used in SEM Secondary slectons are dotcte by the upper SE £2) Outotens ype, 6 Indens type, etector when fis shor, orb the lower SE ©) Soke (seinen ype tector hen fis on, 62. Concerning Evacuation 41) Why must the electron beam path be placed in a vacuum? electrons were to encounter = number fa molecules onthe way twas the sap they woud colle wih those molcules and scatter, whereby they would not esch the sample, To aved sucha stiton, the electron beam path ofthe SEW mest be kept in a vacuum with whith ar molecules are minimized. The distance over which an electron advances ater once calising with 2 certain molec unt the next calsion is called the “average res mation ofthe electron’, and by reducing the presture anc extending his motion a far as posible, te lacon can reich the sample ‘witout contacting an ar molecule. The election beam path ofthe SEM is general ept at t pressure of aound 10° Pa, whereby the “aveage free mation ofthe ecto’ fs about 40 m 2) How isthe evacuation performed? ‘Atypical evacuation system forthe SEM is shown in Fig. 1. Wit a SEM having a thermionic gu, the entre elcron beam path fom elecron gun to specimen chambers evacuated by i uion ump (ODP) or turbo molec pump (TMP), and mainiained ata pressure of 10°19 10*Pa. Ano ( rotary pump (ORP) i utiized for pre-evacuaton at specimen exchange ofr post-evacution inorder {to keep he backpressure of ODP/TMP ow. Aso he electron gun chamber ofthe fd emission 'ype SEM, must be evacuated to anuttahgh vacuum of around 10° Pato keep the sutae ofthe ‘lseton souce clean st an atomic vel. Asputerion pump (SIP) suse fortis purpose, Note ‘thatthe elton beam path contains a numberof small paritoned comparimentsconncted by means of efies, nd a aiferenal evacuation mechanisms uilzed for gradual increasing tho pressure toward the specimen chamber, This enables Keeping the electron gun pres.ie constant leven fhe specimen chamber pressure vais. ‘SEM a cry pump such as sel pump may sometines be used in place of ORP fer evacuation ofthe specimen exchange chamber orpostevacuation. The reason fr thisisto minimize te effec of specmen contamination caused by backstreaming of al vapr fiom ORP. a ( ZI] se onerous) ames — = eae ene xin o \ chamber a ies one 2 hae | or — opPartMP FFU oppor ©) Thormionictype SEM.) Field emission SEM Fig. 1 Example of SEM Evacuation System a3) What are the merits and demerits of each type of vacuum pump? abl 1 gives the operating pressure and mets or demertsof he main vacuum pumps “Tobie 1_ Operating Pressure and Mera/Dements of Vacuum Pun end ofpamp | Operating ers Demet pressure {es ORF ‘Aimosphere |= Usable for preeracuation | Unstable oes presure to | atmos-pheric pressure) applston io" + Simple stuctue and Foor ran is ater age. low-priced ‘Dy panp | Aimoaphere [= Usable forpreevacuaton | Sucre ether complox and (ezotfpamp | pressureto | (atmospheric pressure) high-priced. ste) io = Sites evacusten ‘OOP 101107 | > Rapid evacuation = Some depersion ofa vapor “Nelnose or vibration caused | Require po- and postevaciaton| + Routes wa'r ciler THe 10" 10 | Cities evacuaton * Complex stuture and “nde range of operating high-priced pressure + Requires pre-and postevaciaton oF TO 10 | -Nomecharicalviraion | Evacuation rata sow ‘Low power consumpten | “Requves preevacuaton 4) What kind of maintenance do vacuum pumps require? “The ORP pump require ol exchange once evar sie mont oa yea, tobe cared out bythe user Exchange shouldbe performed using t land method prescribed nthe instucton manval othe pump. Athough other types of pumps have almost no maintenance to be cated ut by te uses, fotow tne purpisruton manual as to tequency of periodical Inspection speci by manufac3. Generation, detection and usage of SEM signals 41) What happens when electrons strike the sample? ‘An electron is very smalin comparison wih he space between the atoms which compose a specimen. Therefore, when an electon penetaos the specimen, tis scattered through interactions withthe atoms. In this process, some of the Incident electrons fy back nto vacuum as bockscatred eecrons (608 2) Fi, butters lose energy while eriting ‘secondary elton Fig 3), ays Fig 3), Sant cathode minescance) eto. ad Analy remain insite the specimen as shown nFig. 1. Incase ofa conduebve specmen, te primary electrons remaining insite the specimen are detected as specimen absorbed) curent ‘The electron dspersion msi a specimen canbe wsuaized by the technique of Monte ati simulston, An example of his vsualzation i shown in Fg.2. This example reveals thatthe ‘der area when ther energy i higher andthe pacman density smal Backacterd Cathodoluminescence Xr Fo Incident electron beam Secondry cecror 7 7" Secondary electon etecer Inside sloctron ‘peotrtion area Interactions between Insden lactone ‘and Speeen Flg.2 Election Seatring inside Specimen as Visualze by Monte Caro Sinulaon 8) Upon inesence of 16 keV on carbon (0) specimen ») Upon nldenceof 1 KeV on carbon (C) specimen ©) Upon incidence of 15 keV on god (Au) spesmen 22) How are backscattered electrons produced?” Backscattered electrons (ls called reflected Necessary information as givon below is clearly expressed, “Topographic information, composienal formation, eyalinfrmaton te “<2 Wrong infomation a given below i not contained Various artacts, damage, extemal disturbance, et <3 Gratin an brightness evel are appropriate. 2) What effect does accelerating voltage or condenser lens current have on image quality? ‘changing the accelerating ‘voage alters the incident elatsnsip betwen Aerating Vella nd Te Qualey lection energy ta specimen. eae “This entails changes of ens aberration (1-5), ae of ons ltd toimeeveatty [Low —— ies ‘leton scattering inthe ieee [Serace Inara 0 ‘pscinen (3-1), secondary “opendatargtvon-pecimen) | sntrmaton nation ‘lection emission yiold(28), Image esttion ag a ‘ee, Inconsequence, varous (penis larson specimen) Image quay changes as shown Specimen damage a InFig era brought about (oends larly on specimen) 3 ‘Terefre, accelerating vl=9® —Cgxtaminaton Basy tome, Sateany to ‘sone ofthe important operating (dopendstaray on specimen) | 22.907 matt ‘parameter for obtaning a good ae ed came, Toten eae legaty onthe substance and Comers us a shape ofa specimen. $0y0U meson fsharserate xray | TD held leo y ‘should se this fue for cosiaten cae reference ony, Fg. Relatonshie between Accelerating Votage Change (Change to aferent and Image Quality in SEM condense excitation currant ‘terse focal eg (1-5) of hanes unis when Varin Caner et Cart is lera Theta changes of rote cant nd probe Conder arc amet (elon beam deter). In consequence, the ntandinfuence | Smat| ——> Laree cantatas = ste pen Sa Cinecagcmseccen Betoeeteete ame Sa Soeviecne aa -FE-SEM (1-3), the probe — — sgl Semcrnavomes Gace ma affected by change of the neem Sciam ‘rs thermionic emission SEM (1-3), “epeMde nes 0 scien) Scieroeaeteness” —g2. meeting Cy Cntr ume ameter of FE-SEM ssa. ‘Asustment ”3) How must accelerating voltage be selected according to the sample? ‘Contato secondary electron image is dependent significant onthe shape, density, et of a specimen, The stuetures of bulk specimens for SEM are oughly clssabe it € categorie shown In Fig. 38)tof). reach category, an accelerating vltage which can be thought be appropriate in generals described. However, attention shoul be pai because an approprsteszceeratng votage * fl. ‘And, becomes positive when = fz * @ at le ele eee | Incase ofa non-conductive specimen, ba z 's almost 210 and ln is determined bythe specimen substance. Therefore, the quantity of le, namely secondary election emission yield (28) dotrmines the charge stuaton, (tote +00 Fg.9. Charge-up Phenomenon on Sutace of Non-conductive Specimen9) How is sample surface potential changed by charge-up? it charge-up occurs the potntal onthe speciman surface changes iowa the postive er negative ‘ie unt the secondary electron emission yield & becomes 1 a shown in Fig. 10. Therefore, the level of specnen surface potential maybe approximate by the diference between the actual Incsent ‘lecton energy andthe incldentelecvon energy where & equals 1 onthe cbcerved specimen, However, the nidetelecron energy where 5 equals 1 varies wih specimen and imaging condtons. Inthe example shown in Fig, 10, ts probable that the potent changes about 900 V toward the postive side when the incident energy is 100 Vand close o 9 KV toward the nogatie sie when the energy 6 10 6, However, he surface potentials not always constant in actual ceses, because tis potent maybe sigicanty dierent aly due toa competed specimen profile or hargngsischargng may be repeated at carta intervals. Fig. 10 Change in Specimen Surface Potental at Occurence of Charge 10) How isthe image disturbed by charge-up? ‘And, how can the image disturbance be prevented? mage robles due te charge-up phenomenon can be sorted into wo fypes;<1> nage dsureance ‘2nd <2> abnormal contrast Ther ae cases where beth types <1> and <2> concur. Type <1> ‘cours as shown n Fig. 11a) because the rasan poston of incident electron besm changes, ‘aflecte by an elect eld caused by charges. This dsturbance arises when the specimen ‘surface charged up ata comparatively hgh potenti. For prevening this disturbance, reducton of ‘he probe cuentas shown in Fig, 11h), owerng ofthe accelerating voage, tc. ae eect. Type <2 occurs as shown in Fig. 122) because secondary electron emission is affect ty the charge-up ‘lected. Incase of 2 postive potent the emitted seconday elections are pe back the specimen se and cannot reach the delete, @ back one appeass. Incase of anegatve polenta a white zone appears, Preventive massure fe basally the same asin , In Fig. 12),