TRNG I HC BCH KHOA H NI

BO CO K THUT PHN TCH PH

TI: Phng php phn tch ph EDS

( Energy-dispersive X-ray spectroscopy)

SVTH: Nguyn Vn Du
Lp: Vt Liu in T
GV b mn: TS. Nguyn Ngc Trung

Tr-ng i hc bch khoa h ni

Bo co k thut phn tch

ph
ti: Ph-ng php phn tch ph EDS
(Energy-dispersive X-ray spectroscopy)

Sinh vin thc hin: Nguyn Vn

Du
Lp: Vt Liu in
T
GV b mn: TS. Nguyn Ngc
Trung

H Ni, Ngy 25 thng 05 nm 2009

Ni dung bo co
1. Khi qut chung v k thut phn tch
ph.
2. Nguyn l ca php phn tch bng
EDS.
3. K thut ghi nhn v chnh xc ca
EDS.
4. Mt vi ng dng ca php phn tch .
5. nh gi ph-ng php & Kt lun.

I.

Tng quan v php phn tch

ph EDX

K thut EDX -c pht trin t ngng nm 1960 v thit b

th-ng ph xut hin vo u nhng nm 1970 vi vic s dng Detector
dch chuyn Si, Li hoc Ge.
C nhiu thit b phn tch EDX nh-ng ch yu EDX -c pht trin
trong cc knh hin vi in t, cc php phn tch -c thc hin nh
cc chm in t c nng l-ng cao v -c thu hp nh h cc thu knh
in t.

S cu to my phn tch SEM ng dng ca EDX

Ph tia X pht ra s c tn s(nng l-ng phtn tia X) tri trong mt
vng rng v -c phn tch nh ph k tn sc nng l-ng do ghi
nhn thng tin v cc nguyn t cng nh- thnh phn.
Ph tn sc nng l-ng tia X hay ph tn sc nng l-ng l k thut
phn tch thnh phn ho hc ca vt rn da vo vic ghi li ph tia X
pht ra t vt rn do t-ng tc vi cc bc x ( ch yu l chm in t c
nng l-ng cao trong cc knh hin vi in t ).
Trong cc ti liu khoa hc, k thut ny th-ng -c vit tt l
EDX hay EDS xut pht t tn gi ting anh Energy-dispersive X-ray
spectroscopy

II.

Nguyn l ca EDS

Khi chm in t c mc nng l-ng cao -c chiu vo vt rn, n

s m xuyn su vo nguyn t vt rn v t-ng tc vi cc lp in t
bn trong ca nguyn t

T-ng tc ny dn n vic to ra cc tia X c b-c sang c tr-ng t

l vi nguyn t s (Z) ca nguyn t tun theo nh lut Mosley:

Tn s ca tia X pht ra l c tr-ng vi nguyn t ca mi cht c

mt trong cht rn.
Vic ghi nhn ph tia X pht ra t vt rn s cho ta cc thng tin
vow cc nguyn t ho hc c mt trong mu. ng thi chow cc thng
tin vow t phn cc nguyn t ny.

Hnh nh ph tn sc nng l-ng tia X ca mu mng mng ghi

nhn trn knh hin vi in t truyn qua.
iu c ngha l tn s tia X pht ra l c tr-ng vi nguyn t
ca mi cht c mt trong cht rn. Vic ghi nhn ph tia X pht ra t vt
rn s cho thng tin v cc nguyn t ho hc c mt trong mu ng thi
cho cc thng tin v t phn cc nguyn t ny.

III.K thut ghi nhn v

chnh xc ca EDS
I.1 K thut ghi nhn

Tia X pht ra t vt rn (do tng tc vi chm in t) s c nng

lng bin thin trong di rng, s c a n h tn sc v ghi nhn
(nng lng) nh detector dch chuyn (thng l Si, Ge, Li..) c lm
lnh bng nit lng, l mt con chip nh to ra in t th cp do tng
tc vi tia X, ri c li vo mt ant nh.

Cng tia X t l vi t phn nguyn t c mt trong mu.

phn gii ca php phn tch ph thuc vo kch c chm in t v
nhy ca detector (vng hot ng tch cc ca detector).

I.2 chnh xc ca EDX

chnh xc ca EDX cp mt vi phn trm (thng thng
ghi nhn c s c mt ca cc nguyn t c t phn c 3-5% tr ln).
Tuy nhin, EDX t ra khng hiu qu vi cc nguyn t nh (v d
B, C...) v thng xut hin hiu ng trng chp cc nh tia X ca cc
nguyn t khc nhau (mt nguyn t thng pht ra nhiu nh c trng
K, K..., v cc nh ca cc nguyn t khc nhau c th chng chp ln
nhau gy kh khn cho phn tch).

IV.Mt vi ng dng ca php

phn tch
1. Nghin cu n mn v l quay xi mng

n mn v l quay Ximng -c chia lm hai loi: n

mn trong qu trnh dng l do ng-ng t hoc hp th
n-c v n mn ( nhit cao) trong qu trnh l lm
vic.
2. Hnh thi v thnh phn ca g st.
Cc sn phm n mn u gin, xp v gn ging
cc. G ch tip xc vi gch chu la c mu nu nht
cn ch tip xc vi v thp c mu nu bng hoc en
ng.

G in hnh. Pha gch chu la: en, nu. Pha v l - sng

bng v en
Phn tch tit din ngang ca g bng phng php SEMIEDX
cho thy g c cu trc xp v a lp - gm nhiu lp k tip nhau
vi thnh phn chnh l oxyt st v sunphua st.
T c th phn bit c ba loi g:
- G khng cha clo v kim
- G cha clo khng cha kim
- G cha c clo v kim

Biu EDX mt ct ca g, Mi biu ln lt tng ng vi O, S, Cl, v K. K hiu

Ka di mi nh l ch tn hiu phn tch c l tn kiu Ka

Phn tch EDX c thc hin trn 4 mu c ly xung

quanh mt v tr: mt mu bt g nghin mn, mt mu g pha
gch, mt mu g pha v thp, v mt mu y ca gch chu
la . Kt qu c trnh by trn bng 1. C th thy rng hm
lng lu hunh (S), clo (Cl) v kali (K) hai mt g rt ging
nhau: S = 3,5%, Cl = 6% v K = 0,5%. Bt n mn c hm lng
S cao hn (c 15%) cn Cl thp hn (ch khong 2,5%). y ca
gch c thnh phn gn ging sn phm n mn. Ph X-ray ca
bn sn phm u c oxyt st v sunphua st vi hm lng
khc nhau
Bng 1. Phn tch vi lng 4 mu ly xung quanh mt v tr (% khi lng)

G st

St Lu hunh Clo Kali

Bt g

74

15

2,5 0,5

G pha gch, mu ti

85

3,5

6,0 0,5

G pha v thp, mu sng

85

3,3

6,5 0,5

Mu y vin gch chu la

56

13

5,5 1,0

. Bng 2 l kt qu phn tch ba mu: bt n mn, g pha v l v

g pha gch. Mt ln na, bt n mn li cha nhiu lu hunh
hn hai loi g n mn tng ng. Tuy nhin g li cha rt nhiu
kali mc d vn cha mt lng clo d .

Bng 2. Phn tch vi lng 3 mu ly xung quanh mt v tr (% khi lng)

G st

St Lu hunh

Clo Kali

Bt g

64

14

12

6,5

G pha gch, mu ti

64

1,5

19

7,0

G pha v thp, mu sng

81

2,0

11

3,0

. Phn tch nh lng EDX vi cu trc ca g

Trn: phn tch nh lng
Di: SEM ca g
biu trn c cc nguyn t O, S v K

Hnh nh phn tch SEM-EDX trn tit din ngang ca g

cha kim. Ln ny cc i ca S khng phi lc no cng trng
vi cc tiu ca O. Tri li, nhng vng c nh du (a)
cng cho cc tn hiu ca O, S v K, trong khi cc lp thp oxy,
cao lu hunh v phi kim ch thy nhng vng nh du (b).
Nhng nh khc ca cc nguyn t ny cng c cng c trng.
Ti nhng vng m cc hp cht ca O, S v K chim u th th
hnh nh rt r nt. Tn hiu ca Cl thng khng i km tn hiu
ca K v S.

V.nh gi ph-ng php & Kt

lun
-u im:
Ph tia X pht ra s c tn s (nng lng photon tia X)
tri trong mt vng rng v c phn tich nh ph k tn sc
nng lng do ghi nhn thng tin v cc nguyn t cng nh
thnh phn.
. phn gii ca php phn tch ph thuc vo kch c
chm in t v nhy ca detector (vng hot ng tch cc
ca detector).

Nh-c im:
chnh xc ca EDX cp mt vi phn trm (thng
thng ghi nhn c s c mt ca cc nguyn t c t phn c
3-5% tr ln)
EDX t ra khng hiu qu vi cc nguyn t nh (v d B,
C...) v thng xut hin hiu ng trng chp cc nh tia X ca
cc nguyn t khc nhau (mt nguyn t thng pht ra nhiu
nh c trng K, K..., v cc nh ca cc nguyn t khc
nhau c th chng chp ln nhau gy kh khn cho phn tch).
Kh nng loi nhiu km hn WDS.

The end!
Cm n thy gip em hon thnh bi bo co v mn
hc!