Im, 111 ,111111 and M 1r11puhtu Mill' ..,, In cht: N.Jn<x,c.

1 % 23

or 111:igncuc ficM~ '111u, dungc I\ '- ommuum de pcndmg on the clccu 1c. and nug11rtJC field E k « ~
1cmcs, "Inch ha\'c Iewer .lhcr riuons than c1cc.trmuuc lc11SC\, .ire used m electron m1croscopy

(a)

(b)

Fig. 2.1 : (a) Intensity distribution at the image plane forming an Airy di$k The point5 are considered resoh-ed
ii the intensity maxima are '>eparated at half the height. {b) Rayleigh criterion of resolutJon.

What does an SEM contain?

The principal elements of an SEM are discussed belov.•.
1. Eltctron g un: The electron gun provides a stable beam of electrons. The mosc common form of an
electron gun is a cherrruonic erruccer, wherein the ,.,.·ork funcrion 01· me metal is m·ercome by che surface
temperature of the filament. Typically a hairpin filament made ot a run~cen wire of tOOµm. wnh a op
radius of 100 µm, is used co generate electrons. The filament is held at a neganve potentul 2Ild he.ued to
about 2000-2700 K by resistive heating. The electrons are confined and focused ~· a gnd cap (\Vdmdt
cap) held at a slighdy higher negative potential than the fibmenc.The confined beam 15 accelerated co che
,mode held .tt the ground potential and a portion of the beam is p.a.ssed through a hole. The be.am current
measured at the anode is used co regulate the power supply which dnves che electron gun for the ~
currem. The tungsten wire gradually evaporates due to the high operaung ternper:ature. Its ttStSUnce
~ecreas.es and finally it becomes so chin chat ic breaks. Higher temperature (higher opn.anng c:urttnt
increases the evaporation rate and reduces che filament life.
The filament characteristic is given in terms of brightness wluch 1s {;1\'t':ll as current ~~~olid ~ngle.
T~e brightness is of the order oft<,s (A/cm 2 sr) for che tungsten filament. An order of nu~umde mcre;iscd
?nghtnes!> h posc;ible in the case of lamhanum hexahoride (LaBJ-b.ased guns :and a sull b.I"b~r bnghmess
~s p~ssible in the case of field emission bruns. This 1s aclueved by reducmg the enussion area.,, luch resulcs
m significant reduction in the demagnification reqmred m the oper.mon.
 Lan h,h lm.~.Hl't b1
ii hl nc ,, i \ hfct1mc as compa
.,
,\l\ll ., ongc ten T h e emitter
. h . redrotountungs
ti
,_ ,., t .. \ ll ,a \\ n \l \0 µ m d\ is a sing
"' " \ .\l nl .'l t'I w 1l \1 C,00 µm
length 1 e up ts .
d to a sharp po in f 10 µ m led
the- 'l ; ,ta\ i, m<> N m
tc
d on ., themum I bo n
· b T h gb"ce is resist to
d h th .
an
t"nut, ckcm.,n, or gt .,p uu c L,
ase e ....., ively he at e so t at e tip
1 he ~ m require, lt h:~ ,~ceded for a h ·
he- , on ta nu na tc d .l bc tt ct v~1c
uu~1 1 tungsten filamen
th an t as
llMific-. an order ,e
c~,1h. T \ h.,,une t I1femnc is of t d
n ·
the or er o f 10 00 h an d th e increased
t e_ ti p can
bn gh tn ess
of mJgnitude incr
ease m cost.

variable rnamen
t power supply

Filament

Wehnelt
cylinder Bias
(Grid cap) resistor

High
wltage
~
+

~~
\ cunertl.

Beam current
Anode Plate

Fig. 2.2 : Schematic o f an

electron gun. The gun is
implies regulatio normally operat
n of th e current ed at a constant
<Ref. 1). supplied to the filament. emission current,
Adapted from J. which
I. Goldstein, et al. (2
003)
1=idd em m io n ill
another way o f m
emis!>ion, the field akmg electrons. T
at the tip of th e en his kind o f source
electron emis~ion utter reache,; a mag has a high brightne
geb reduced and nitude o f 10 V /n ss. In field
Two kind~ o f field become'i narrowt'r m, and the potent
e111ission -.ource, so th at el ec tr on ial barrier for
field emitter (Sf£ ,m• rnmmonly us can tunnel and es
). In c 1=E, a !>harp t'd, i,t'. the cold cape the cathode.
single cry,t.1\ of < field emitter (CFE
T he tip is made o 310> tungsten tip ) an d th e SchottkY
f tu n~ te n as it ha is spot-welded o n
the tip.The tip its s the \trcnbrth requ a tu ng
elf is mounted m ired to w it hs ta nd the sten wire.
a triode configur mechanical stress
ation so that the produced at
potential differen
ce be tw ee n the up
 l11wstig,1t111g ,111d M,1nip11l,1ting M;it,:ri:il~ in lhc Nanc,sc.:ile ~ ,I,'
25

· · ·1ne potenu·a1 dI ffierence

.m d tlw flt ,t l'll'n rod<• i, of t hl• or de, of , 5 r.1 V to procJ uc:c 1,J µ A emm1rm. ··
·· · · ·
I'('t\\"('t·n lht· ,t·cond decuo . 1•<I t IH:. lip t Ietermr·nes the be,,m energy. held emJSs1on is sensm ve ro
d"' •1,
8th Mhed ~-1\t~, •11 ~d tht· ,urf.tu.· <,in lw cleane d by flash mg the tip to a tempe rature of250 0 K.After fu.shin
g.
· covered . Th e np L-
· h~ to uc re-lU3"--hed
tlu· l'm1,,H)11 1, IHgh but ,non it reduce , and •tab , 1J1zcs as th c $LI rf:ace is
• ·
• J J1ours o f operat ion . In each fl ashing, the t1p gets more um ;an
bl d
1 'l't J ck·.m ,urfact · ;)(T\111 ar.Lcr
10• r-. ' i:,• •
11 •cv
' era
has to be change d.This occurs only
at_ca ,eve r .ti thoma nd, of flash~s, the trp is render ed unfit for use and it
after several years as one flashing 1s enoug h for a day.
their tips sharpe n in the e:xtr.iccion
SFE.s are operat ed at high temper atures. They are self-cleaning and
n barrier . The rip is held ;at ;a high
field. In SFEs. the field at the tip is used to reduce the work functio
n, the surface is coated wfrh Zr0 2
tempe rature. In order to achiev e better reduct ion of the work functio
t is drawn . This keeps the ~ ~em
from a dispenser. The SFE gun is run contin uously even when no curren
oir is finite, the lifetime is finite and a replac ement is neede d every
ye2r.
clean . Howev er, as the Zr02 reserv
copy is shown in Fig. 2.3(;a). This
2. Electron lenses: An electro magne tic lens used in electro n micros
in an iron casing. A magne tic field is
cons1Sts of a coil of wire genera ting a magne tic field enclos ed
h the coils. The electro n in a magne tic
genera ted betwe en the polepi eces by applyi ng a curren t throug
tic field reverses after the center of the
field underg oes rotatio n. As the radial compo nent of the magne
n leaves the lens \\;thou t any net c ~
lens, the rotatio n in the first half of the lens is revers ed.The electro
the axis. Since the radial force is directe d
in the angula r mome ntum, but it underg oes deflec tion towards
n travelling off-axis to the beam path
toward the axis, the magne tic lens is always conver gent. An electro
which the beam starts bendin g to the
will spiral throug h the lens toward s the optic axis. The point from
focaJ length can be varied by chang ing
point where it crosses the lens axis is called the focaJ length . The
lenses where the focaJ length is tixrd.
the curren t in the coils and this is a differe nce from the optical
Refer ring to Fig. 2.3(b), the focal length can be given asf= 1/p
+ 1/q. From this.on e can calcula te the
magni ficatio n, M = qlp and demag nificat ion, m = p/q, where
pis the distance from the object to the
of the lens.
centre of the lens and q is the distanc e from the image to the centre
nser lens has a large bore giving a
An electro n micro scope contai ns two kinds of lenses. The conde
axial extent giving a short focal length .
long focal length , while the object ive lens has a strong field ofshort
c curren t passing throug h a condu ccor
resulti ng in high magni ficatio n. In an electro magne tic lens, an electri
id (several rums around a cylind er),
gives rise to a magne tic field. If the condu cting wire forms a soleno
centre . The flux density :u rhe center is:
each turn contri butes to the induce d magne tic field at the
1~s c~e num~ r o~rurns._J is_thc
B = µ(M //), where µ is the perme ab~ty of the surrou ndmg mat~rial,
id. H_ - ,\Ill_ and so b} suhsn tu~,
curren t flowin g throug h the coil and / is the length of the soleno
B = µH. So, µ is the flux densit y per umt field. For air and non-m agneti
c matenal~. µ = and B-1.? f!·
The perme ability of iron 15 field-d epend ent and 1t is unity at high
field and ,o, B = H.At high magne nc
d I ti • reason why µ = 1• Due to the hvstere sis• of iron, the
· · • • .
fi eIds , iron reache s magne tic satura tion an t 1at 1s 1c
used to _get the lens char.actensncs s~ch as
extent of curren t used to energi ze a magne tic kns canno t bt.·
for this rc.ison. ~he ~urrenr_ results m the
focal length . Hyster esis has to be kept small and soft iron 1s med
The ~ystem 1s shielde d. trom extern al
heatin g and coolin g by water is neede d to keep the system cool.
magne tic fields. For this, a high perme ability materi al is used (
µ metal LS one such material}.
 2b

\\ hc-11 tht' st~k llll.td a, CnLa,t',! m ,t ca,;c ,,f,Pll mm, tlw 11 1,1gnl'llC tidd ,dong I he.· ,1.xi-; is inrrc,i~cd If
the
:mnu I.u
!,!a}' 1, 111,hu.· nl ,nit 11011 ••1 gn:,ttc.·r ro11cc1Jtr,1tio11 of the Ill
•

J
1

~-
~ , ,"ICU <"Xl'X'pt .at a n.in'l1\\
1 • •

;ignetic
ltr'd
,'t
-'·
Iii.fl.'\.:~ "-
~nort
..
a:\."l.lll d1<.ta1h~ ou ur,.1 he .
,,,,1,·ra-c,·,
.u,· tht·,t• .111nul.1r rinh" which focus the 111.1gnct1c
. .
.
• _..., • typi cal imtrum cnt~.
lbou at .a ~,~n IOC'..1t1on.111~ held ,tn'u~>th u,,·d 1, bd,m· 20.()()() g.tus\ 111

ObJect

f q

- -- - ~ - - Image

(a) (b)

are shown. (b) Illustrati on

Fil} 2.3 : (a) Schema cic of an electrom agnetic electron lens. The magnet ic field lines
oithe concep t oi magnifi cation.

tically correct ed
The foal Jengrh is given by f = Ki, (., '1)2 w here K 1s a constan t; v, the relativis
aooele nnng ,'Olcige; and /\/1, che numbe r of rurns of rhe coils. Focusin g is achieve d
by varying the current
to current . The foc.tl
throug h che coils. le is impon.: rnr ro nore char rhe foca l len1:,rrh 1s not Jiuearly related
is affected by
Jeng-Ji of die lens is directl r propor tional to che accelerating voltage . So the image quality
\."2I)'JJlg me electro n \'eJocit}~

there is no w.iy w
Lnu cbtn:m.ons: Electro n optics suffers from abc rr.ttions . ilur unlike in light optics,
sohc diese :aberr.m ons.AIJ chat can be done is ro rt.>d uc:e them through proper
design conside rations.

more strongly. As •1
SphnicaJ aba,-atJ01t: Eleccrons 111 far away tr:ijecrnne:. frnm tlw optic axis are bent
different spot
rc:suh. the electron beam emenn g the lens ucar d1c edge of the lt·ns, is brough t to focus at a
~ the SJ>OtS closer to the centre. ~l his is schc111 ,1t iL·ally rnustnated in Fig. 2.4(a). The error in the image
axis of the lens.
u.e to this become s rnore pronou nced as the uc:1111 is 111ovcd furth t'r .1way from the optical
 Im es1 g t n and Man pulat ng Mat rials m the Nanosu 27

DiffC":-rnu21 focmm!? ousc, the unage at the penme,er to £f, smeued ~ d of 1: the ttntre As a r •
0
~ ~ ; lb: mu~ 3 Pt'('.:l~ 25 3 dBk ~ld not as :a pom: The ~mall~t disl 1s called .he sphenal abttra·
di i-: 0 • le~t con,''\Non. d, = 1/2 Ca \\ here C 1s the sphenol aberr.ioon coeffiaen: and a IS the angle
of the ourer m cluou;h the leru. C, 1.5 typically :a tew mm for lm.-e5 with shor. foal lm.:-.hs The sphenul
abcrnuon cw be nururruzed by removmg the ou.er edce of die beam. This 15 acruC\·ed by placin£ a small-
holed aperture ,lt che centre of .he nuc;ne~c field or ~'lledu..e}y belaw 1,. Ho\\C\-er. :a muller du.me·e~
miuc~ the beam cur-rem 211d ilia leads to aperture dtffi.tcnon.

OrrMWiU abm.;w.n;: This abernnon is due to the eneq~·y spread of the electrons. \l/hen li~ of c:li:E"r.-e,r
energi~ eme~ a converging lens ;u the ~e po1m, che extem of ddlec.:ion will depend on ~ie rner-g-,. ln
light opcio. r.diarion ot a shorter wavdeD.£Cb 15 deflected more strongly .h.an ~ of :a lon,;er '\"\'J\~lrng-.h.
In electron opacs. che re\"erse happens. 1.e. a ~honer ,u,-eleng-..h is ddiec...ed l~ woru::h·.This IS due .o .he
t"".h.-c .hat elecrroru .ue subjected to les.ser dedecoon when th~ beam energy is hi£h.. ~:s·.
resuli. die be.ams
of ~"O diE"erem energies form inuges .u cliferenc poincs as illuscra~ m Fig. 2 ..!(t>). Due ,o chis 2ber.-a::ion.
Ul.Stead oi , point. a dtsk results and che du.merer of ilie disk o: le~c confimon cm lbe ;i,-en as.
J = C a (1 EI E.). where C IS the chromic aberruion coefiiciem. E. is t h e ~ ene!Ff :and !1£ is :he
enerm spread. The fracriorul ,-ariar:ion in beam energy IS the significant iaaor.
Chronucic aberration cm be reduced by subilizing the energy 0£ :he elecrron bewi. Sr.wilizcd
accelennon \"Oh:age and impIU\-ed gun design enstL"'C che s:.lbi!i..-y oi ciie i:>eam.. 11'le e::ec oi ch..-ommc
~rracion i.s pronounced near the perimeter oia converging lens and an aperrure an be used w dimim:e
these elearons.

Apmurt d,ffraaion: The wave nature of elearons 0.1..1.ses the beam to diffi::act upon pming through a
rurrow slir. &ch beam passing through che slit Sets up ics own ·waves. These will incena: co gn-e 2 bright
spot in che middle and a ser of concencric ~ in che inuge plane called the ·Air)· disk·. If the intensm
discnbution is plotted in one dimension. ic looks like due one sho-..m in Fig. 2.4 c). The concn'buaon ro
the spoc size due co dilli-acrion is given as die half dimiecer oi die Airy~ d1 = 0.61 }. / a , where A is
che waveleng--..h of che beam and a LS che aperrure half angle. In order co reduce rhe dfea:s of dttfurnon.
it is necessary t0 have as greac an angle as ~1ble be.ween che opnol 1-'0S md the lens pmmner. Tlut
would amoum to having no aperrun: ar all. Bu: a smaller apenure is needed lO reduce the dfecn of
sphencal aberration and chromaric aberration. wtuch would cause diifracrion problems.Thus m oprunum
aperture size must be chosen.

AJcigmacism: Asrig:nmism refen t0 the; improper sh.ipc oi che beam.:\ pomt obJeet is focused co two-
line foci at the IJ'i'Uge pbne and UlStead of a point. m elli~ appem. The rwo-line foa DU} be fort't'd ro
coincide for correcting this defecc. A.srigrrurum occun due co defera m die foamng lidds. which could
be due to severa.l ~peccs reb.ted co elc:ctromagnecic lenses, aperrurt1 and omer column components.
Imperfection in nuchining an ause 21ng.numm. Asrignumm B cometffi by :.a set of nugnm ailed
'srigmawrs', which are placed a.round che c1rcumfrrencc of d1c column These att adjusted :.acronhng to
mength and p01ition in an effort co mduce an equal and opposite etfeCl on the ~
The effect of lens aberrations is import.mt for the obJtCO\"'t lens :n the dferu aUSttl to the be2m
would be mull in comparison to the diameter at ocher len.ses.Typ1o.J sphencal :.abm.rion can be corrected
 ~o et poi nt p Object point
. , '
, , '' '
..
, ,
,, ''
''
''
,, , ''
, , ''
, ,, '\
A
,,
a ,,
• Bea m at the
per iph ery 1s
bent mo re
Imago Ima ge
pla ne pla ne
Sph enc al Chromatic
abe rrat ion aberration

(a) (b)

Ob jec t point
Ob jec t

Len s

len s -all~-
Disk of least
Image
pla ne ......._,.,_,......,. confustion
/'-- - Diffraction
pat ter n Line focus 2
(c)
{d)

rration,
gn efl c lenses. (a) Sp her ica l aberration, (b) chr om ic abe
of e/e rtro ma
Fig. 2.4 : Various ah crr ati om a'iliRmatism. Ad ap ted from Golds
tein, et al. 20 03 (Ref. 1).
re ddfr,1( tio n, ,m d (d)
(c) ap cnu

uld be con tro lle d

lea ds to ,1p crt urc dif fra cti on and the ref ore the se tw o sho
com ple tdy . But tl1l· co rre cti on tage of 10 kV.
rom ati c abe rra tio n is sig nif ica nt bel ow an acc clc rat mg vol
propt.•rly. Ch d
the sca n coi ls. In SE M, the sca nn ed im age is for me X
t of the SE M com ist s of r. th
J. ~ " coils: Th e ne xt par
. I . n co1 l s. T J1cre are tw o pai.rs of coi.ls, on e each a:or e ,
po mt by po int a11d t h c. sca n 1s ac 1a: vcd by the sca
 Investigating and Manipulating Materials in the Nanoscale %, 29

and Y axes (Fig. 2.5).T he scan coils lie within the column and
move the electron beam as per the requirement
across the specimen. They are electromagnetic coils and
are energized by the scan generator. The scan
generator is conne cted to other comp onent s such as the
cathode ray tube (CRT ) and the magnification
module.
Th~ scan is made as. follows. The electron beam swept
15 across the sample. The patte rn over the
sample lS synchronous with that observed in the CRT. The
secondary electrons produ ced by the sample
are detected. The intensity of the signal at the CRT is propo
rtional to the secondary electrons. An intense
signal can illuminate several dots on the screen, while
a weak signal would mean that no dots will be
illuminated by the electron gun. The detec tor therefore
gives the intensity of the signal, wlule the raster
pattern gives the location of the signal. In this way, the
image on the CRT is built up point by point to
match what is happe ning on the surface of the sample.
This mann er in whic h an image is formed is the essent
ial difference between the transmission and
scanrung types of microscopes. A couple of impo rtant obser
vations need to be made in this type of image
formation. Firstly, the focus is depen dent upon the size of
the electron beam spot. The smaller the spot on
the sample, the bette r is the focus. Secondly, magnification
is not produced by a magnification or enlar gmg
lens but rather by taking advantage of the differential betwe
en the size of the scan pattern on the sample
and the size of the CRT.
The size of the CRT is fixed.The size of the scan pattern
on the sample is variable and is deter mme d
by t~ magnification module. By narrowing the size of
the area which is scanned and conveying that to
the CRT , we can increase the magnification of the image
. The smaller the area scanned, the lesser is the
distance betwe en the raster points, and the smaller 1s the amou
nt of current needed to shift the beam from
point to point.The greater the area scanned, the lower 1s
the magnification, while the greater the distance
between the raster points, the greater is the amou nt of
current needed to shift the beam from point to
point . In this way, when we operate the SEM at relatively
low magnifications, we actually push the scan
coils to their extremes.
The scan gener ator changes the step curre nt to the scan
coils. This curre nt is then multiplied by a
constant by the magnification modu le and sent to the scan
coils. The higher the total magnification, the
lower is the multiplier constant.

4. Electron detector: There are two lands of electrons comin

g out from the sample in an SEM; the
backscattered electrons, with high energies being larger
or lower than the primary beam energy, and the
secondary electrons whic h have energies of a few eV, or less
than a few tens of eV. The most comm on kind
of detector used in SEM is the Everh art-T hornl ey (E-1)
detec tor (Fig. 2.5). In this, a scintillator material
is exposed to the electrons. Energetic electrons, upon impac
t with the material result in photo n emission.
The photons are transmitted throu gh a light pipe. This is
a glass rod or a piece of plastic. At the other end
of the light pipe, a photomultiplier is placed, which converts
the photons to electrons through photoernission.
The electrons can be made to under go a series of collisions
on surfaces producing a cascade of electrons
and a gain of 106 can be achieved this way. The detec tor
has a high bandwidth, whic h means it responds
to a rapidly varying signal. This woul d be the case when
the primary beam is scanned over the sample at
high speeds.
 '

Sea coils

~ Sea:, gen!."lt!On •

~~~- ...... -~-

Ff\llape rue
, /atpAU pom
~~:Jid e
E-T Detector
,_ __\ •l2kV ' Backscattered electrons

~ t --- --~
I
L
-!/JV to •250V

Fig. 2.i : Smem.J!,c OI an 5£\l The electron beam r, sc,anned b) a ~11015Cm ro,l, andthes«ondMyelec:tron5
t dereeted b) the cktecr0t. 8\ apph ng a negative potenllal to the Faraddt c• ~ secvndM)
,:-J.,.-rm,,.,..· ,a t: ,eyeaed comp!ert l. Adapted trom Goldstein
et ,1/. 2003 (Re,: IJ.

e pru'tla l opn.uo n ofthe.- dc.-tl"('tor, :a chm m(U) c~nng as applxd on me u6ce al'dat•
•Milac•-:
,-c potc.-ntul ts :applied to the.- mml surface so that all d«trons. induding die b, ~
not 6t tbt
tttro an- accdemcd to 1t so as to generate photons ~ high wkage should
.and fj r dm rc~son. a faradJ\ age 1s kept over the santilbcor, which as aecaicabaulalrd.
• desired potfflw1111 th.: range of -50 co +250 V to the Faraday CJF, a con.-. 111 m,n or

r stt'Orubn dc."CUOns bc."comes possible.

u.x~•-" 4; ha k:sontted decuons, a sc-p.,me deceaor an b e ~ Snenl
....,••111
•
~
f the more popuhr ones is the solid sure diode dtt«tor. This wora • piaaplt
1inllll:Xm auctor the dcctron unp.tct on produce dectron -hok
paan if the . , . _ Wlgy IS
rt-no<hok !. nlue "tuch rs of the order of a ft'\\ eV. Thus,
whffl a high CDalJ . _ . ill OIi 11.
1Cb(IJU<~ncl:1 of dccuo, -hole sum are fonncd The chargn can
be Swtpf m ~ clMdDM if.a
e dwge colic tcd can be :unphficd and detected
\EM, the e,ommon demon dececcor as the channel pbre lfffl. rl I I llillaon5
a d and a asade of sec:ondaf) d«crons as produced. Scwal IUdi -1 l F b1"'
 Im 1 111 i\11111 rnd M 11111ml 111111 M 11t ,, ti, In rht N ,nr ,I, u

11,t\ l'll 1 ,t,,l "h11 h ,, a h" drn11it ll i, ,rnd du <let ,nm,< 0111111 i 0 111 11 th oth r 11d u
l 111 111
I \ I l\)'hh ,1 I\, llH 'l \ Olllbt \ cit I I Mil ) ,rhl llll I( I \ ( ' Ill tlH low ) (, V ,11,wc, lw111 I pl It t ork
"' h,11,\\ 11111~ 0 1i11.i11011 l u" 111r1n) 'liimd u ) dttllrnl, H;q 11 m: 1ctclc1 111 n11 lor cl C Cllfl byJ
,!111 nd ,,1n11

\t M: Modctin Ad, ancrs

,1 M h thl mt~,, ,, 11lr-h 11 ' <'ll t k, 11, 1 11 1111110\111p11 1,·, h1111i11 e I Im" I11gc:ly h ec,111\C of its vcr,JUhty, m
\o&rl\lm mr,rlr'~ ,,j llllllflll~. 1',"1' ,,f s,1111J'l1• I'" 1•,11.1111111 , po~\l hrhl) ol ~pc, r,,1ltopy ,11cl d1tTr,1t1io11, as well ,1
<'ll•\ mtc-1 pt'{"tatton ,,1th, 11n11~!r,, I lt1• 11111h11d " ·" l11rh rl11oughp 111 111 ,tlllg 1t ,111 1Ct:c~~1blc fac.1hty A \cry
" dr t'llll,.--C ot ma~mfir:.llu, ,,, 1, ,l\ ,1il,1hh· "h11 Ii 1111 ,l11,11c~ rlw \ 1rn.1lr, 1111m 111 v irtll ,lly every dct,111 Bc,t
,1 M, dut o\,tim unag, h i,"'111111 1m 111 t lie 1,111g1• 111 11 S 11111 .111«1 fnr tlm, the ~ 111,plc need not be spcc1.;ally
p 1'fllrNI SJlmplr s1rr is 11111 a 1111111.111;) 11 111 .S l· ~1 ,111d ,,,111plcs t\ 1,11 •,w 11" ~i111 n11 v.,tfcrs c~n be put directly
m II morlrm 11uH h1111
Modnn ~ch11111 c,i SI Ms 1111h1t• f11•ld l' IIIM11111 ,11111\ n.'I 111·11· 11.1\l' hcc11 ri11111ero11\ 1dv:111ccs 111 \,1nou;
l~t~ of the h1rd\\ .;a1e,11, h ~, l1•1N·,, dt tl'11111, ,111d d1g11,tl 1111.11:W ,H q1m1t1011.'l ltcst· ml~nc<.~ in h;ud\\Jre,
C'ouplcd \\ 1th ad\lUH 1•~ 111 11tlH· 1 ,11 t'," 11i 111\1111111t·11t.1111111 su l h ·" pnwl· r rn ppli,·\, lugh ,,..cuum
anstnunMuauon h;i,r 110\\ 111.11h• 11 p11s,1bl1• 10 ,1tq1111t· \ I M 1111.tgc, frn111 almmr ,1nytl11ng, mcludmg \\et
h10I01g1cal ~mplr,
Lo\\ ,olugc- SIM•~ ,lll11d11•1 11t·w d1°H·h1p111t·111 .'I ltt· l'\lrt·111t• ,urftl'l' st:11rn1v1ty of tlm tcchruquc 1~ a
r~uh ol die reduced m1r1:a1111111 \'nl11111t·. ·1Im .1ll0" ~ tht· IIH',l't11t·111c111 of 1111.1gc, \\ 11h nanometer scale
~ohmon wnh under I kV ,11 t t·ll'1 .1111111. A1 tl1t·,t· 111" t' t1t·1g1n, rl1.11gt11g 1s not ,111 1m1e and 1t as po~s1blc
rn mc-a~uf'C'm1.tbt"S "11hou1\11111h1111H' 1n.11111g,.'I lw t·b11011 t·11t·rgy r,111 bl· n:d11l·ccl further by appl)tng
a neg1m-e potenu:d <.111 1he \,1111pll· ,111d 111 tl11, ".1y. till" lh·,1111 l' lll'I gy l ,111 he rcd11cl'll co bclov. I 00 eV It
al,o mil,<"~ ultni lo\, , o lr agt· SEM (UI V \I M) p1M1hll'. wh1d1 ,, t'\ltt'llll'lr ,urt~11.:c-scnsmvc and a\01ds
beam mduced damage :11 su1 la1·t•, .
\Jihcu an dccuon ht·.1111 11Ht•1,1lh w1rl1 111,tttl'I, 'l'\l't,1l p1mt'"l'!I lll111r. Tlwse result m particle or
s1oton cnmsion proccsH'!i "l11c h .m· ,11111111,111,t d 111 hg ~.1,. ·1 hl· l'lt'l tron t'111h,1n11 procco;;;es mdude
cbi.uc.: and mdamc ,i;c:1 11\ 1111g, ;rnd dH· l't111"1011 of 'l"t 1111d.11 }' l'ln trom .111d Aur:a cltctmns. Inelastic
f.atu"rmg OOlUa .i, the h(·.1111 1111c,.11 I\ wirl1 thl' ,.1111p lt· ,111d t·ln·11011it t'M 11,ll1t111, lll tht.' commuent atom~
an o ur Thoe cJ;c11.i11om <an ll•,111
111 ,·,rlt·11t l' ,111d I otl' l'lt·t tw11 l \1 ll,tlll>tl, ,1ml t>IIUNCin. I hl· core hole
thu rellted flU} get filled h}' l·le< 111111 dt·•t'Xt 11,111011, 1n11l1111g 111 , 1 1y~: 1 ht· dt>- t''i:l 1t,1t1on can al,o remit
m de uou CJecuo11 , c.illed J\1ig1•1 1·1111s\11111 . 111 .1dd11i,111,, 11111\11111 111 1ht· prn111n bc.•am can .ll\o lead co
c-x 11..iUon ofluucc \1hra11m1s, ,...II d1t•i,t• l'lt•ct 11111, l,111 lw 11,l·d 111 M.llhl'I 111tlt11\r11p1< 111fornnuon ofthc.-
UmJ le In add1wm, du:) r..11 1 :il\o hi' 1m·d 111 11li11111 1 lt1·11111 ,,I u1 l 11111p1"iu1111.tl 111~1rn1,u1011 .,, 111 the c.1~,·
ofAu(;;cr d cuom 01 muctm:i l lllf<11111:11111111h 111 till• l,1\1· 111 li.11kM ,1tt1•H·d t•lt·t tllHl, In .1 norm;1I SEM
1maJ;c, 0111> 6C oud;uy dectmus ~11 r dc11•1,;1cd. I 111"s111m 111", li.11.111c·11\t1, X l'il\!1 u~ \\di as contmuom
XU)• 0<cur I he d121.ictc 11UH X '")~ a ,,. usrd 1111 qu,1111,111\1' 111d q11a11111.111\\' 111lurmmo11 In ,1el,ltt1on
to lh<$c, elecuon 111 dmld dr),ur J>LHl11, 11111 , WC1h111, <u ., nl~11 ill, 111
J i11,;h rc-~oluuon :,1 M 1s 111m a a11111111· 111ml ) u, ,iii 1111 ,I 111 11;11111\\ It'll! 1• ;111d tl•l h11uluh'), tlm hcn11ncs
an m1J>01t.1m l11glt 1hio111~1p1H cl,a,,H tt, 11.1111,11101)1 l1 as 1111po1 1,111t 1( 1 knu\\ llw duncfl'ilOlls ofthe m\leture<i
 n·~ . T hu s SE M
'l'Zln:'d wl wn , h.u ·.1, t\'I il 111g dc \•ic c \C r uc tu hl' c:o,11 e.,
h l'"
fahric-Jtt'd and tht' m ,tr na i11g 11.m o, l'.tlc: c.1Jib r.1t ion ).
111 mcc:r,,1,)gv (., ln .u1 (" h im ,,lv
narw
mdiTC"INtblt" t,>o1

Prima ry electron beam

lon sra tom s Ba cksca ttered ele ctr on s

I
Auger electrons
Ch ara cteris tic \ -•avs

Secondary electrons
ContmUOlis \ -•avs

Sample

Heating , sample damage

xe!>se:,. in the sample.

fig. 2. 6: Ekcrron be am -in duce d prc

Mi<nwaalysis l resoluti
io n nu cro an alv s1s of ma cenals is possible. Th e spatia
hig h spa cia l resol ut citat:Ion beam, wh ich is of
the order ofi
fn bo th SE.i\1 :m d TEJ\1 . all dim en sio n of the ex
,:-.i b]e by rh e <:m us excitations in
of cb e an aly sis is nl 3d e po ms tru me nt s. T he ele ctr on be am causes vario
fev, na no m et er s in .-.t3 te-
ot:.rhe- ar t
sen t in the ma ter ial . Ch aracteristic X-rays emitted
pre
lcrer i,cfr of th e ele me nts identification. Th e int en sit
y of th
su np le. wh ic h :u-e c.har. be us ed fo r ele me nta l
co re ho le de ca v ca n
th e sa mp le as a resuJ r of
cit3ci\-e an ah -m . y dispemv
si,gna.1 an be us ed fo r q u:m rre sp on ds to the en erg y analysis called 'energ
m cwo ways. On e co elength dispersn:
f\1 ..ia oa iul ys :is is do ne .sp on ds to wa ve length analysis called 'wav
ile th e oc he r co rre em
~ m er ry " (E DS ). wh uc ion 1s po mb le in W DS , it is mo re cumbersom
hi le im pr o\·ed en er gy re ,ol or tio na l to bo th th e energ
y JIJ
sp ea ro rn ea y• (U 'D S) . \~' m the de tec to r 1s pr op
S. In ED S. J si~'llal fro ray are de ter mi ne d separa
tely.
am e- co ns um m g du n ED en gth an d in ten si ty of the X-
me X-'n,·s. In ~ ' DS, rh e wa \·d
- Th is results ·
mt cn sm ., of
. m. it ge e, de ce ler ate d du e to the co ulo mb ic field. 0
ch es rh e aro to as bremsstrahlung
U' :he n 2n de co -o n ap pr oa erm · ap pe ars as ph ot on , ref err ed
ch e ele ctr on an d rhac en
1
.a Joss of en er gy fo r all en erg ies rill the en erg y of th e or igi na l dectr0'.
s of
l'.2d iario n con rains ph ot on electrons. Th e characteristic
X
'br ea ki ng nd iat ion -_ Th is en eq,> '}· of the pr im ary
as an d. ea ro n aa n los e ~m
y en ergy, fro m ze ro to rhe thl y \~ Jry ing ph ot on intensity. Th e«
J
s on chi s far ge . sm oo
D) 'i em .m ed by th e
ato ms will ap pear as sp ike n be ide nti fied. Th e intensities of the
se Jin~ cJ
an aro m c.r
\• lin es wi th wh ich tho ug h various pa ram ete rs
deterru in
se ve n) du r:u u: ris oc X- f3 g .. pe cie !> in rhe sam ple .
be related to d1e concen
tr.acions o f di e em itt in ion int t·nsity are, in ne r shell ion
iz.ation Cf\)),'
ace d ro X - ray ern hs
ru m asp ects ref
the imcnsmcs. Th e im po o f ma terials an d X- ray pr od uc
tio n range.
tio n cro ss se cD on
s.cction, X-ray ab so rp
 fnH hgattng :ind Ma111p11lc11ing \\atcrial~ In the N,mosrnlc

1 Elh a pllonm, emnted l" the sample a, r collcucd ,111d mc.m,rccl su1111ltanco11~ly
hy a §Ohcl ~Ute
K'42\ &tectu~ llu~ oommon EDS dc1r~tot ,, l11h1t1m d11ltnf ,,Ju 011. S1(I 1). l111r1m1c or high punty Ge
iPGc u al~ used, wfuch ~ nrnrc l o1n111111111t tlw <~~col r I M umnmH·11t~ due to then higher (;ullccuon
dnOO'K"\ \Vhen an X-n, photon fall, on ~11 11Hr m,ir \C1111rnndtH tnr (h.1vi11g no (;h,1rgc c~rr1cn), due to
ph ~puon, durge camcn (clcl lJ\111, .md hole,) arc crc.1tcd. 1 hc\C .ire \Wept by ,111 :1pplred bi:u
a du.--ge pul,;c illu, charge pul,c i, then rnnwrccd imn .t volt.1gc qb'fl,11. lmran~ic con<lmort 1s hird
w aduC'\'t' md det~ctor c.rpuh arc m.idc lo bch.1w hkc intnn,ic ,,)icon. J'hi, i, m.1dc hy Jpply111g [ 1 on
p-cype ~Ulet:bv fomun~ .1 r -nJUllltion.Thejunct1on region will behave ltkc m intrin,ic \ertuc.:onductor.
The " ~ ot dmrregion c.m be e,~.mdcd by applying :an electric field at elevated temper.icures. The
l'CD0\':21 o, most o, the p-tyt"e ~1 re~1on m.tl.:e\ a detector (which i\ the 51 left behind). l lowcver, the Li
present u mobile at room temperature and it is ncce,\arv to cool down the detector 10 77 K in order to
ope.r.te the detector under bi~. '
The w:rmsic ~con acove layer i) covered on the front 5idc wnh /Hype S1 ,rnd in the b.1ck with 11-
npc Si.The front 15 :abo coated ";ith a tlun gold layer for electncal concact. The device is kept behind .1 Be
wmd°'" aiuch bloc.1.s visible light. Also, it mechanically seals the detector assembl~ from the vacuum
dumber. thereby :n-01ding contmunaaon. When an energetic photon strikes the detector, ch.irge earners
~ OC2ted. The detector is rever~e-b1ased, 1.e. p--type 1s connected co negaave potential. This means that
,._,1icn the durge carriers are created. the holes move to the p-sidc while the electrons mow co the ti-side,
thus ~ g a pulse of eleco-ons at the 11-s1de, which can be amplified. Jn order co reduce noi,e and also
Li mobilit)~ co m.a.imair1 the intrinsic condmon, the detector 1s cooled. When photons of high energy
2.bo-."C the S1 K sheU binding energy (1.84 keV) fall on 1t, phocoeleccron emission c.1ke, plJce. The
pbcr..ode.co-on loses enerb'Y inelastically, thus excmng electron-hole pairs.The core hole produced may be
fi!kii b-y phoroenussion or Auger emission.The photon may be reabsorbed resulang m phoroemb~ion, or
11 m.zy undergo ine!a!ric scattering.Thus, ail che energy of the initial photon is used 111 gen er-a ting electrons.
In fn'OUnbJe conditions, che number of charges created in the detector per photon i, equ.tl co photon
energy/energy required for che creanon of an electron-hole pair (e) For a 5000 eV photon, chi, works
out to 5000/3.86 or 1295 electrons (e ac 77 K is 3.86 eV for Si). However, chis number i, wry ,mall.and
gener.ates a \ery small charge:: pulse of 2 x l 0 H, C. Each charge puhe, convened ro voltage, repn·~enb the
ent"rgy of the- photous. The resolution of the photon energy, d1stingui,hablc by solid ,c;lte detc:-ctor, of this
i,
ldnd,is 130 eV 2c MnKa {589() eV).The detector re,ohmon a funrnon of X-ray ener~y .rnd it i~ about
65 eV at 282 eV.'Jltere ,n: sevtraJ advanced detecton ~uch a, rht' \llt<.011 dnfc <let:tt.•rcor, "hid1 \\mks at
250 K, having the s:une rt~oluriou but an mcrcased s;tmplmg rate. A m1croc.1lorinwtt•r U)\ \\llrks b)
measuring the temper.Hurt: differtnce camcd by the absorpnon of X ra>, WHh thi', un 111cre.hc.>d ent"rg)
resolu □on is possible, wluch 1> about 4 5 eV at MnKa.
Wavdengp, dispersive spec1rcm1t:te~ work 011 the pr•11( 1plt' of Br.1gg ditfo1c1io11, ;i,l ::: 2.d,1118, "hC're
A. 1~ the w,velength of rht X- r.1y .111 d 0 I\ the J11glt' of 111t 1dt•11t l' l ht'1l'lun-, .11 \ ',1mHI\ ,111gll♦, lit 111c1dcnce,
tt 1~ pos~ible to scatter rays of diffortllt wJvde11htth~ to thr dett't ma A, ,1110 l .llllllll ht' l;.u~c•r tlun one", the
long~t wavelength diffracted h 2d, thcrcfon· the t I y~t.il put, ,1 ltm11 011 tlll' 1.111gl' llf l'lt·mt'nh l li,-en•d
There are also other limfrations of the han.Jwa,e. Wlieu O 1, 'JlJ'>, dtt' dt•tt•no1 h.1' ll 1 ,u ,It the X ray
source; when sm 0 15 close to zero, the movcuitut of tltl' t 1) ,c.tl 11t-.11 tht• \Pl'l llllt'II 1, ,1 l*'bll·m. In order
to diffiact the low energy X-rays emitted by ilc, B, C .111d N, it h lll'l'l'\\,11 y ru 11\l' t l r~t.11~ of l.1rgl' d, alues.
 34
0
.,, ~ poss h c b\ L:mgmmr-Biodg ett films (,ee che chapter on )elf-assembled 'Monoldyers) L
h
~ f f ' s p ~ an be CW1ed br ,-an,ng che ch.am len!-rth of the monofaver. ;\ltosr of th \\· oSc
-i-~ • d , e measure
ot - -":n ...-A-Ue~ X-r.n-s are one b,· • Ln-ered
• . svnthetic
• . microscrucrures .This co n ca·ms evaporated alteIllents
tn-cn ct ht:-l'-.. .md light demems. The duckne:5.s ot the byers can be e.isiJy controlled. ~te

~ dtteao:- commonly emplo;1='Cf i, a -t..>a.S proportional counter· This h as a gas rruxture · ( ·

Or per an: . i . . ~ l O per ~ot mcdi~e). The detector a.s,emblv has a thin \"\ · d . chr gh ~picaJJy
• .,,-., - .c.n_ . • - • ,n ov.: ou which th
X-rn ~~on u.us m. le ouse-.s the e;ecoon ot, phocoeJectron • \vhich 15 • acceJeraced by che high vol e
~-J..
on .::
the- coileaor.
.,..s - chi
The electron c.n15es ,ub,equem ioniz.-a:ioo in ch e gas and as a res uJ c, a gam fact uge
o~ Ul~ o..d'r o! Iv 15 a • t"\-ed. There fu,·e been numerou,· improvements m .
· gas-fill e d d etectors mvol · or
-L- - •
uu; use O: ~I'O'-a: w·r.ndc-'L.., cdier gase--. ere. Vlng

Th: 5P4ml resolution I ;·SE\I is ~ecred by the beam size as menc:ioned before. Bue the beam causes
th ch . .
m:~-oon w·1 e ~ ~ ...n..l the region of interaction exceeds che physical dimension of th b
mcre-..ses J..uer.tllv as ,veil as depth-wISe, and .L:. c ·
ui.u m eracnon vo1ume
e eam
d epends
:rad:. The
J.._ d _e~ent
--=-•cf>4tul __ • on
w:r nu:cu.i • an 1
ii.DU • on .he beam enerP"\,•
_ •::,r i \r larg · th b ·
e energ1es. e earn mceracr.s to a greater extent, while
ch-: dqd1 ~f 1m·eacno~ d ~ ~,~ch a decrease in elecrroo energy till about 100 eV and at ve low
energies o.: die o.-der o.r a ~e'\'-" e \~ It mcreases again. The range of interaction is decided by the e17ctron
~ ~ o n 1en;-...h. The uruversa.I electron acreouac:ion lengrh of materials IS given m Fig. 2.7. As seen m
me tr_gu.:-e. die a~e-nw.non leng-..h increases "ich electron energy and has a minimum at a few hundred v
This nu.k~ ir possible co design highl·.- surface-sensitive SE.\11.s by reducmg the beam energy. T~
~--dopmen~ is discussed in low energ", SE\.1.

2 2 2 Transmission Flectron Microscopy

ln TEt\1., the a.msmirred electrons are used co create an image of che sample. Scattering occurs when the
dec.uon beam inceraa:s with marrer. Scarrering can be elastic (n o energy change) or inelastic (energy
change). Ela.sric scaaering can be boch coherent and incoherent (,vich and without phase relationship).
Ebsoc saaering occurring from well-ordered arrangemenr.s of atoms as in a crystal. results in coherent
sci.we-ring. giving spot pacrerns. This can be in che form of rings 111 the case of a polycrystalline material.
Hov.~rer,. mdasric sc.aaering also occurs. which also gives regular patterns as in the case of Kikuchi
pane-ms. Jneb.sric processes give characteriscic absorpcion o r emission .specific to the compound or element
or chemical scrucrure. Because or" a1J chese diverse processes, a crammiss1on electron microscope is akin co
a complete labor:2cory.
There are t,.VO main mechanisms of conrra.sr in an image. The cransmitted and scattered beams can be
r.ecombmed 2t che image plane. chus preserving their amplitud es and phases. This results in the phase
romrasc muge of [he object. An amplitude conrrasc image can be o btained by eliminating the diffracted
be2It1S.This JS achie\·ed by placing suirable apenure~ below the back focal plane of the objective lens. This
tnuge JS cailed che bright fidd image. One can also exclude a1J o cher beams except the particular diffiactc.-d
bc.:m of mterest~ The image using chis is called che dark fidd im age (Fig. 2.8).
TEMs v.rith resolvmg pov.ers m the vicinirv of IA are now common. As a result, HRTEM is one of
'
the mOSt ~senual roo1s of 112noscience. I nceraccion · 1as · d
of the electrons wah rhe ~ample produces e oc an