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Alicatiun uf Atuuic lurce Micruacuy

un Farticle Characterizatiun
Alicatiun Nute
Maozi Liu,
Agilcnt Labs
Jing-jiang Yu,
Nanotcchnology Mcasurcmcnts Division
lntruductiun
Farticlea, eaecially nanuarticlea are
uf great acientifc intereat hecauae their
ruertiea change aa the aize aruachea
the nanuacale. 1he ruertiea include
utical, uagnetical, uechanical, electrunic
and therual ruerty etc. 0ue tu thia
unique feature, nanuarticlea nut unly
attract uuch attentiun fruu the acientifc
cuuuunity hut alau are hecuuing
uure and uure iuurtant in ractical
alicatiuna auch aa cuatinga, data
aturage, catalyat and nanuelectrunica.
Nanuarticle characterizatiun ia a key ate
tu underatand nanuarticle'a ruertiea
and tu cuntrul the uanufacturing and
alicatiuna. Nurually nanuarticle
characterizatiun eaecially aizing, ia
dune hy a variety uf uethuda auch aa
light acatter uethuda, aediuentatiun
uethuda, electrical ruerty uethud and
iuaging uethuda. Fxcet the iuaging
uethud, all uethuda ueaaure article aizea
indirectly, aince the aize ia interreted
haaed un a uudel ur a theury fruu auue
ueaaured arauetera. Auung the
iuaging techniquea, utical uicruacuy,
electrun uicruacuy and acanning ruhe
uicruacuy are the uain techniquea.
0tical uicruacuy can unly he alied
tu ueaaure articlea with a aize larger
than une uicrun. Flectrun uicruacuy can
ueaaure articlea duwn tu nanuueter aize
in vacuuu cunditiuna, while the aaule
rearatiun ia cuulicated.
Scanning ruhe uicruacuy, uainly atuuic
furce uicruacuy (AlM} uffera aeveral
advantagea in article characterizatiun.
lt ruvidea 30 infuruatiun ahuut articlea
aize. lt ia caahle tu ruvide uther
infuruatiun auch aa article ahae, aurface
area, electrical ruerty, ruughneaa and
cheuical cuuuaitiun in uuat caaea. With
the uwerful data ruceaa auftware, AlM
can alau ruvide atatiatical arauetera uf
articlea auch aa the aize diatrihutiun, area
diatrihutiun, vuluue diatrihutiun. Mureuver,
AlM can characterize articlea in different
envirunuent including air, vacuuu, liquid,
aecial gaaea, elevated teuerature, luw
teuerature etc. Cuuared tu electrun
uicruacuy, aaule rearatiun ia eaay.
Saulea can he cunductur, aeuicunductur
ur inaulatur.
Caahility uf Meaaureuent
uf Farticle Sizea with
high Satial 8eaulutiun
AlM haa a very high reaulutiun
(auhAngatruu} fur ita ueaaureuenta
in Z directiun. 1herefure, even auh1nu
articlea can he ueaaured accurately
if they are uaitiuned individually un a
Nat auhatrate auch aa uica, which ia
atuuiclevel auuuth.
ligure 1 ahuwa twu aaulea uf iaulated
nanuarticlea iuaged hy AlM in AC uude.
0ne ia a cell lyaate, which ia an inaulating
hiuaaule. 1he uther ia cunductive guld
cullidea. 1he culura un the iuagea
rereaenta different height. lur a detailed
ligure 1. AlM height ueaaureuenta un a hiulugical nanuarticle aaule (left} and an inurganic
nanuarticle aaule (right}. 1he tu ruw ia the tuugrahic iuagea (5 u x 5 u left and 1.2 u x
1.2 u right} and the huttuu ruw ia the curaur ruflea uf the linea un the AlM iuagea reaectively.
8|ze 6haracter|zat|oo oo Iso|ated Naoopart|c|es
8ubce||u||ar 8tructures Au Naoopart|c|es
1opogra
30 |ew
he|ght
functiun alluwa uaera tu cuuhine all the
data flea and get an uure rereaentative
article aize diatrihutiun hiatugrau haaed
un a larger enaeuhle.
Caahility uf Meaaureuent uf
Farticle Sizea with Wide 8ange
Muat uf cuuuercial AlM inatruuenta have
a larger acan range in lateral directiuna
than the vertical une. lur exaule, the
large Agilent AlM acanner tyically uffera
a 8u hy 8u later aize in XY directiuna
and a curreaund 5.5u in Z axia. lur
very hig articlea eaecially thuae having
a aize larger than acanner Z range, aize
characterizatiuna are atill alluwed fruu
AlM atudiea. ln thia caae, articlea ahuuld
he reared un the auhatrate in auch waya
that they are cluaeacked un the aurface.
lur articlea which can furu acked
uunulayer un aurface, Farticle aize can
he deteruined hy ueaauring the diatance
hetween twu neighhuring articlea, ti
cunvulutiun duea nut interfere with the
diatance ueaaureuent un XY directiuna.
ligure 1 ahuwa aeveral exaulea in which
all the articlea are cluaely acked. ln thia
caae, the aize range that can he accurately
ueaaured deenda un the lateral
reaulutiun uf the AlM and the acanner'a
acan aize. lur a acanner with a acan aize uf
1u, the article aize range that can he
ueaaured ia fruu <1nu tu 5u.
2
and quantitative analyaia, a curaur rufle
can he extracted fruu the data. We can
clearly aee that the lyaate articlea having
height ranging fruu 2nu tu 6nu. lur guld
nanuarticle un ailicun wafer, the curaur
rufle ahuwed that the articlea are
unifuru, with a height uf 6nu.
Additiun tu the accurate ueaaureuent
un Z directiun, AlM alau deliver a high
reaulutiun and accuracy in XY directiuna.
Yet fur iaulated articlea, it ia uure
accurate tu ruhe their aizea haaed un
the height than the lateral ueaaureuent.
lntrinaically, AlM iuage ia a cuuhinatiun
uf the ti geuuetry and the aaule
geuuetry. ligure 2 illuatratea thia ti
cunvulutiun effect. Clearly, the lateral aize
uf ia ti aharneaa deendent. A hlunt ti
reaulta intu a larger lateral aize, and a ahar
ti givea a lateral aize cluae tu the real une,
while the height uf the article reuaina the
aaue in huth aituatiuna.

While AlM ruvidea the highreaulutiun
ueaaureuent at aingle article level,
enaeuhle ruceaaing ur atatiatical data
analyaia can he achieved uaing uwerful
article analyaia tuul auch aa the Agilent
AlM data ruceaaing auftware Ficu luage.
lur exaule, atatiatical infuruatiun auch
aa article cuunting, uean article aize and
article aize diatrihutiun can he achieved
quickly. Farticle aurting hy criteria auch
aa area, equivalent diaueter, urientatiun,
aaect ratiu, ruundneaa ia alau availahle.
ligure 3 ahuwa an AlM tuugrahic iuage
uf a aaule Al
2
0
3
. y uaing the data
ruceaa functiun eak cuunt hiatugrau",
we can get the quantitative height
diatrihutiun uf all the articlea within thia
aecifc iuage. We can alau exurt the
hiatugrau aa a data fle. ln the caae that
uultile iuagea were taken at different
lucatiuna uf the aaue aaule, thia
ligure 1. 1uugrahic iuagea uf auue cluaely acked articlea with a diaueter uf 1nu, 3nu,
9nu, .5u, 3u and 5u, reaectively.
ligure 2. Scheuatic drawinga illuatrate ti cunvulutiun effect. ligure 3. An AlM tuugrahic iuage uf Al
2
0
3
un uica and ita curreaunding aize
diatrihutiun hiatugrau (right} generated hy Ficu luage. Scan aize 2.1u x 2.1u.
uaot|tat|ve Aoa|ys|s oI a Fo|yd|spersed 8amp|e (k-A1203, 25 om)
8|ze 6haracter|zat|oo oI 6|ose-Facked Naoopart|c|es
1nu Silica 3nu Fulyatyrene 9nu Fulyatyrene
5nu Fulyatyrene 3nu Silica 5nu Fulyatyrene
uechanical (atiffneaa, frictiun} and
adheaive ruertiea uf aaulea. 1herefure,
it ruvidea a ueana tu ruhe the uateriala
cuuuaed in nanuarticlea. ligure 6
ahuwa the AlM iuaging uf a aaule, that
cuntaina twu tyea uf ulyuer articlea
with different aizea and uateriala. 0ne
ia uly (hutyl uethacrylate} with a uean
aize uf 128u. 1he uther ia a cuulyuer
(5 hutyl acrylate\ 16 ulyatyrene\1
uethacrylic acida} with a larger aize uf
217nu. 1he uixing uf huth articlea
un aurface haa heen verifed hecauae
tuugrahic iuagea (lig. 6A and 6C}
clearly reveal the cuexiatence uf the twu
tyea uf articlea with lateral diuenaiuna
curreaunding tu their characteriatic aizea.
1he aaule ia iuaged frat under luw furce
with a uruae uf hetter viaualizatiun uf
the tuugrahy. under auch cunditiun,
Nanuarticle Shae Meaaureuent
lur the characterizatiun uf articlea,
article ahae analyaia ia hecuuing
uure and uure iuurtant in additiun tu
article aize. varying the ahae uf the
articlea reaulta changea in the aurface
area drauatically. Since the aurface area
deteruinea huw faat a cheuical reactiun
uccura, article ahae ia an iuurtant
araueter in the haruaceutical and
cheuical induatriea. 1he uuat cuuuunly
uaed technique fur ahae analyaia ia
iuaging technique. 0tical uicruacuy and
1FM ruvide iuagea that are 20 rujecta.
Althuugh SFM ia ahle tu ruvide a 30 view
uf the aaule, it ia very diffcult tu get the
true value un the vertical directiun. AlM
uffera viaualizatiun un three diuenaiuna
with auhnanuueter reaulutiun and
reciaiun. ln ligure 5, a fher like ailicun
nitride nanuatructure and a rectangle
ahaed Yttriuu 0xide ia ahuwn.
Caahility uf Material 0ifferentiatiun
ln additiun tu the unrecedented high
aatial reaulutiun, anuther key advantage
uf AlM ia the aiuultaneuua uultichannel
data acquiaitiun. ln AC uude, tiaaule
furce interactiuna cauae changea in
aulitude, haae and the reaunance
frequency uf the uacillating cantilever.
1he aatial variatiun uf the change can
he reaented in height (tuugrahy} ur
interactiun (aulitude ur haae} iuagea
that can he cullected aiuultaneuualy.
Fhaae aignal ia very aenaitive tu the
3
the difference in haae aignala hetween
twu tyea uf articlea ia negligihle
(lig.6} aa the tiaaule interactiun ia
nut atrung enuugh. With an increaaed
iuaging furce, the uaterial aenaing ia
enhanced drauatically au uany auall
articlea exhihit a uuch hrighter cuntraat
with reaect tu the larger cuulyuer unea
(lig.60}. 1he uhaerved haae cuntraat
variatiun ia due tu the intrinaic naturea uf
uateriala. 1he cuulyuer ia aufter than the
FMA (1he 1g uf Fuly(hutyl uethacrylate}
ia 3 , while that fur the cuulyuer ia
2 C}. 1herefure, haae iuaging
diatinguiahea the tyea uf uateriala due
tu the different hardneaa.
Shuwn in ligure 7 ia anuther exaule tu
further deuunatrate the AlM caahility uf
uaterial differentiatiun with higher aatial
ligure 5. 1uugrahic iuagea uf a SiN nanuuwder, acan aize 3.6u (left} and a
Y
2
0
3
nanuarticlea, acan aize 2u (right} un uica aurface.
ligure 6. 1uugrahic iuagea (A,C} uf uixed ulyuer nanuarticlea
and the curreaunding haae iuagea (,0} at different iuage furcea.
Scan aize 3 u x 3 u.
ligure 7. AlM tuugrahic (A,C} and haae (,0} iuagea uf ulylyaine
cuated 5 nu Au culluida (tu, acan aize 6 nu x 6 nu } and 15 nu Au
nanuarticlea (huttuu, acan aize 2 u x 2 u} un uica.
1opography Fhase
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1opography Fhase
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120om 120om
400om 400om
6ore
8he||
! "
# $
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# $
600om 600om
600om 600om
Silica Nitride nanuuwder Yttriuu 0xide nanuarticlea
AlM lnatruuentatiun fruu
Agilent 1echnulugiea
Agilent 1echnulugiea uffera highreciaiun,
uudular AlM aulutiuna fur reaearch,
induatry, and educatiun. Fxcetiunal
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utiuizatiun uf innuvative and eaaytuuae
AlM technulugiea.
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Fruduct aecifcatiuna and deacritiuna
in thia ducuuent auhject tu change
withuut nutice.
Agilent 1echnulugiea, lnc. 28
Frinted in uSA, March 31, 28
59898211FN
reaulutiun. ln thia caae, huth cunjugated
and uncunjugated guld nanuarticlea
aualler than 2nu are atudied. ligure 7A
ia a tuugrahic iuage uf 5nu catiunic
culluidal guld uudifed with a ulylyaine
cuating. Since the urganic layer ia aufter
cuuared tu the uetal cure art, the
uuter cuating aeara aa dark ring in the
curreaunding haae iuage (lig.7}.
ligure 7C and 0 are tuugrahic and
haae iuage uf uncunjugated 15nu Au
nanuarticlea fruu a hlank exeriuent. Aa
exected, the haae iuage duea nut ahuw
a different cuntraat at lucatiuna uf article
edge. lt cunfrua that the ring atructurea
uhaerved in ligure 7 are aaauciated with
the ulylyaine cuating.
Cuncluaiuna
Atuuic furce uicruacuy ia an
indiaenaahle technulugy fur uaterial
characterizatiun hecauae uf ita veraatility
and unrecedented aatial reaulutiun.
lur article aize analyaia, AlM ruvidea
accurate ueaaureuent uf articlea
ranging fruu 1nu tu 5u at aingle
article level. Meanwhile, atatiatic
inveatigatiun uf a large uulatiun uf
ulydiaerae articlea ia alluwed uaing
article analyaia uudule in advanced
auftware. AlM ia alau caahle uf uaterial
aenaing, which uffera tu differentiate
variuua tyea uf article ur identify the
heterugeneuua cuuunenta within the
individual article.

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