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PH IN T QUANG TIA X X-RAY PHOTOELECTRON SPECTROSCOPY NGUYN L CA PHNG PHP

KE (measured) = h (known) - BE - spec (calibrated) BE = h - KE spec BE:nng lng lin kt ca in t ph thuc vo nguyn t (Z) KE: ng nng ca in t quang, spec: cng thot ca ph k Bng cch o ng nng ca in t quang v bit nng lng ca photon ti th BE c th xc nh c BE chnh l c trng cho tng nguyn t do cc thng tin c th nhn c: thnh phn ha hc v hm lng ca chng, trng thi ha hc cc nguyn t c mt

Cc in t quang pht x su t 10 n 12nm (tnh t b mt mu) c th vt qua qung ng i trong mu v n c thit b. su ln hn cc in t quang s khng th vt qua qung ng ny do mt nng lng. Do d XPS l phng php phn tch thnh phn ha hc trn b mt vt liu t 10-12nm chiu su.

CU TO V NGUYN L HOT NG CA XPS

Gm cc b phn chnh: ngun tia X, h thng thu knh, detector nhiu knh

Ngun tia X:

Anode c ph Al hoc Mg vi dy c 10 micromet cho tia K tng ng vi 1486,6 eV v 1253,6 eV. Hai catode c t v 2 pha v c th la chn mt trong 2 to tia X. Th tng tc l 15KV Tia X to ra c n sc ha bng n tinh th thch anh nhn c K . Tinh th v anode c t trn vng trn t tiu to chm tia hp v tiu t ng trn mu (0,8mm).

H thng thu knh v detector

Cu to gm 2 bn cu ng tm, c hai bn cu ny u c t th m, trong bn cu ngoi c t th m ln hn. in t quang t mu qua mt h thng thu knh tiu t ti khe vo ca b phn tch bn cu ny CHA (concentric hemispherical analyzer), in t t khe vo CHA vi nhiu gc khc nhau. Hiu th gia 2 bn cu xc nh mt nng lng c gi l pass energy. Ch nhng in t quang c nng lng bng vi pass energy mi i vo c CHA v n c detector rn khe ra, detector s m s in t cng nng lng ny Gia khe vo v mu c t mt li vi th m c nhim v lm chm (hm) tc nhng in t quang c cng nng lng i qua ty thuc th m t vo li, nh vy mi mt gi tr ca th ch cho mt lot cc in t quang cng nng lng i qua

ghi c ph ngi ta gi nguyn hiu th ca hai bn cu, ch thay i th m t vo li. Nh vy nng lng ca cc in t c xc nh bi th li hm v hiu th gia hai bn cu.

PHN TCH THNH PHN HA HC V TRNG THI HA HC B MT MU Mi nguyn t ha hc c mt tp pic c trng trong ph in t quang bng cc gi tr ca nng lng lin kt c xc nh bi ng nng v nng lng photon ti. Nh vy BE chnh l du hiu nhn bit s c mt ca cc nguyn t c mt trong mu Php nh tnh c thc hin mt cc t ng bng cc so snh BE vi cc gi tr BE c lu tr trong database ca cc phn mm phn tch ca thit b

Vic nh lng cc nguyn t ha hc c thc hin nh


sau:
S XA IA X = FAB IB XB S IB

IA

IA v IAS l tn hiu t nguyn t A trong mu v mu chun IB v IBS l tn hiu t nguyn t B trong mu v mu chun Mu chun: lm bng nguyn t nguyn cht c cho km theo thit b hoc t cc s liu c trong phn mm phn tch c thit lp trc FABX l tha s mng Vic xc nh din tch pc cn c thc hin sau khi tr nn (loi b nn)

nhng th mnh ca XPS. Khi hai hay nhiu nguyn t kt hp vi nhau to thnh hp cht th s trao i in t s xy ra, iu ny lm thay i nng lng lin kt ca in t mt lng nh, dn n s dch v tr pic trong ph v c gi l s dch ha hc (chemical shift) Dch ha hc ng dng ph bin xc nh lin kt C vi cc nguyn t khc trong nghin cu vt liu polyme, nghin cu tc ng mi trng i vi b mt kin loi v hp kim, v rt nhiu cc ng dng khc trong nghin cu trng thi ha hc ca b mt: phn ng ha hc b mt, tng tc ca cc nguyn t cy ghp v.v

Xc nh trng thi ha hc ca b mt mu l mt trong

To profile chiu su (depth profile): s dng chm ion Ar bn


ph b mt v bc dn tng lp nguyn t v ghi nhn ph XPS, c th thu c s phn b nguyn t theo chiu su ca mu

Profile chiu su ph XPS ca oxit to thnh trn thp 20%Cr, 25%Ni-Nb sau khi b oxy ha trong mi trng CO2

NH IN T QUANG TIA X

c trang b thm mt h thng thu knh to nh v detector to nh, phn gii t 10 n vi micromet

Cu to ca thu knh t C hai cch to nh To nh tng t nh knh hin vi quang hoc s dng chm tia X mnh qut trn b mt mu bng cch dch chuyn mu, tn hiu c detector to nh ghi nhn v th hin trn mn nh Bng cch la chn cc in t quang nh b phn tch nng lng ta c th nhn c nh ca mu, thit lp bn v trng thi ha hc v nguyn t b mt

nh C 1s nh F 1s nh cho thy c s nhim bn C-F trn b mt polyme

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KT LUN Pht hin c tt c cc nguyn t vi Z=3 tr ln (khng th pht hin H v He) Gii hn phn tch c 0.1%, c th t cao hn nhng yu cu thi gian phn tch rt di Phn tch b mt vi chiu su c 10nm To profile chiu su v hnh nh b mt, hnh nh trng thi ha hc b mt ng dng cho tt c cc nhm vt liu kim loi hp kim, polyme v silicat

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