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TP CH PHT TRIN KH&CN, TP 9, S 9 -2006

NGHIN CU CC THNG S TI U CA MNG TiO2 V SiO2 CH TO MNG CHNG PHN X (AR)


L V Tun Hng, Nguyn Vn n, Hunh Thnh t Trng i hc Khoa Hc T nhin, HQG-HCM
(Bi nhn ngy 13 thng 04 nm 2006, hon chnh sa cha ngy 25 thng 09 nm 2006)

TM TT: Mng TiO2 c ch to bng phng php phn x dc, v mng SiO2 c ch to bng phng php phn x rf vi cc nng oxy khc nhau: 30%, 15%, 12% v 6%. Tnh cht quang ca mng c xc nh qua php o truyn qua UV-Vis, cu trc mng c xc nh qua php o AFM. Mng c ch to vi nng oxy 6%, chng t thch hp nht ch to mng 2 lp chng phn x trong vng kh kin. Mng chng phn x AR c th gia tng c truyn qua thm 4.5% so vi khi cha ph mng. 1. GII THIU

Thng thng cc loi knh thy tinh c chit sut khong 1.52. Khi chm nh sng chiu ti vung gc vi b mt ca chng, th mi b mt ca knh s gy ra phn x khong 4-5%, nn nh sng sau khi truyn qua knh (qua 2 b mt knh) s b gim i khong 8-9%, iu ny khng p ng c yu cu trong cc ng dng quang. gia tng ti a truyn qua khi nh sng truyn qua knh, ngi ta thng dng mng mng ph ln knh, chng hn nh mng ph cho thit b thu nhn nh sng trong t bo quang mt tri (solar cell), mng chng phn x trong ng tia catt (cathode ray tubes) . Mng mng mt lp c th c s dng to ra phn x bng khng, trong iu 1/ 2 kin chit sut ca mng phi bng cn ca chit sut [2], n mang = (n de ) . Trng hp c chit sut l 1.52, vy chit sut ca mng phi khong 1.23. Trong thc t rt him c vt liu to mng tha mn c iu kin chit sut ny, cht MgF2 thng c dng c chit sut khong 1.37 (ti bc sng 550 nm). Trng hp Si (100), chit sut ca n kh cao khong 3.85, th vic chn vt liu mng vi chit sut thch hp c nhiu thun li hn. Tuy vy, mng mt lp c nh gi l khng hiu qu ch to mng chng phn x AR. Mng 2 lp vi chit sut cao v thp c sp xp xen k gia cc lp dng to mng AR rt c hiu qu. Chng c th to c phn x gn bng khng ti mt hoc nhiu bc sng. m rng vng bc sng c phn x bng khng, ngi ta thng dng mng 3-4 lp, hoc nhiu hn. Cc vt liu ch to mng a lp thng l cc cht in mi hoc bn dn nh : Ta2O5, PbTe; Ge; CdTe; ZnSe; ZnS; YbF3; YF3; MgF2,; CaF2, BaF2 Trong nghin cu ny, chng ti ch trng vo 2 cht in mi TiO2 v SiO2 v cc l do sau y: Mng TiO2 c rng vng cm ln, chit sut cao, chng thng c dng ch to cc thit b quang in (photovoltaic), thit b quang xc tc (photocatalysts) hoc cht in mi trong mng t in. Ngoi ra, mng TiO2 trong sut trong vng kh kin v hng ngoi, hp th trong vng t ngoi, nn chng cn c s dng cho cc ng dng quang hc nh dn sng (waveguides), knh lc filter hay ch to mng AR. Mng SiO2 c chit sut thp, chng cng thng c s dng ch to mng a lp quang, dng lm lp bo v cc thit b silic, chng try sc trong cc loi knh eo mt v cc ng dng trong cc thit b in. Ngoi ra, mng TiO2 v SiO2 rt bn vi s tc ng ca mi trng, chng li l nhng vt liu kh ph bin, vic sn xut chng c gi thnh kh r. Khi kt hp 2 mng SiO2 v TiO2 vi nhau, chng c bm dnh rt tuyt vi.

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Vi nhng u im vt tri ca 2 mng TiO2 v SiO2 nh k trn, trong bi bo ny, chng ti nghin cu ch to mng TiO2 v SiO2 trn thy tinh v xc nh cc thng s ti u v tnh cht quang v cu trc ca chng. ng thi, cng vi s h tr ca chng trnh m phng mng AR (chng ti trnh by trong [7], [8]) chng ti tin hnh ch to mng AR 2 lp.
2. THC NGHIM

Mng 2 lp AR c ch to trong h chn khng Univex c 3 ngun phn x: 2 ngun phn x dc v 1 ngun phn x RF. Mng SiO2 to bng phng php phn x rf t bia gm SiO2 ( tinh khit l 99,99%) v mng TiO2 c ch to bng phng php phn x dc t bia kim loi Ti ( tinh khit l 98%). Tt c cc mng c to trn thy tinh. p sut nn l 3x10-6 torr, p sut lm vic l 1x10-3 torr. Mng c to trong hn hp kh Ar v O2, vi t l oxy l khc nhau. Khong cch gia v bia l 45 mm. khng nung nhng do s va chm ca cc ht nng lng cao nn c duy tr nhit l 1050C. Cng sut phn x l 90W. Tnh cht quang ca mng c xc nh qua php o ph truyn qua trn my UVVIS-NIR. Cu trc v b mt mng c xc nh bng phng php AFM (atomic force microscope).
3. KT QU V BN LUN

Vi phng php phn x magnetron dc khi s dng kh phn ng oxy th iu kin bn ph v trng thi plasma ca h s nh hng rt nhiu ln cu trc v tnh cht ca mng [3]. Do vy, trc tin chng ti kho st s nh hng ca nng kh phn ng oxy ln tnh cht quang v cu trc ca mng TiO2 vi t l kh oxy c thay i l 30%, 15%, 12% v 6%. Chng ti khng to mng t l kh oxy nh hn 6% l m bo y hp thc oxy trong mng, v ch to c mng trong sut. Nu mng TiO2 vi hp thc oxy yu, th mng c tnh cht giu kim loi Ti v c hp th ln. Ta c th ng gi s b hp thc oxy ca mng qua mu sc nh trong bng 1 [4].
Bng 1. Tnh cht quang ca mng TiO2
Oxit TiO Ti2O3 Ti3O5 TiO2 TiO2 TiO2 TiO2 TiO2 Trng thi n tinh th a tinh th a tinh th a tinh th Anatase Brookite Rutile Rutile, 1000 C
0

Mu sc Vng (golden yellow) Tm m Xanh Trng, , nu , nu en v trong sut Trong sut Trong sut Trong sut Trong sut

Chit sut

2.554 2.616 2.616 2.5

Mng do chng ti ch to trong sut, khi so snh vi cc s liu trong bng 1 chng t chng y hp thc oxy. Vic mng trong sut cng c th hin trong ph o truyn qua nh trong hnh 1.

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TP CH PHT TRIN KH&CN, TP 9, S 9 -2006


100

O TRUYEN QUA (%)

80

60

2 3
40

20

(1 (2 (3 (4

) ) ) )

3 1 1 6

0 % O 2 5 % O 2 0 % O 2 % O 2

300

400

500

600

700

800

900

1000

1100

1200

B C S O N G ( n m )

Qua hnh 1, ta nhn thy tt c cc mng u c truyn qua kh cao khong 90%. Tuy nhin chnh lch gia nh ph cc i v cc tiu ca chng khc nhau, chnh lch nh nht mng (1) vi O2 30% v tng dn ti mng (4) vi O2 6%. Nu dng phng php Swanepole ta c th tnh c chit sut ca chng v ta c mi quan h gia chit sut ca mng vi nng kh phn ng oxy nh hnh di,
2 .4 4

Hnh 1. Ph truyn qua ca cc mng TiO2 c to cc nng oxy khc nhau.

2 .4 2

2 .4 0

Chiet suat

2 .3 8

2 .3 6

2 .3 4

2 .3 2

2 .3 0 4 6 8 10 12 14 16 18
2

20
2

22

24

26

28

30

32

T le O

/A r+ O

Hnh 2. S thay i chit sut mng theo t l kh oxy

Chit sut mng TiO2 s gim nh khi tng t l oxy , t 2.43 i vi mng c t l oxy l 6% gim xung 2.31 i vi mng c t l oxy l 30%. Vic gim chit sut ca mng , theo [3] l do khi t l oxy cao, mt mng s gim v d dng hnh thnh cc l xp. Ngoi ra, kt qu tnh ton cho thy, chit sut ca cc mng trong hnh 3 ti bc sng 550 nm, thay i khng ng k v xp x khong 2.42. Chit sut ca chng hu nh khng ph thuc vo thi gian phn x. Khi so snh kt qu ny vi cc tc gi khc [5] ta thy chng tng i ph hp.
100

80

2 1

O TRUYEN QUA (%)

60

3
40

4 1. 2. 3. 4. 5. 40 50 60 70 de phut phut phut phut t h u y t in h

20

200

400

600

800

1000

1200

B C S O N G ( n m )

Hnh 3. Ph truyn qua ca cc mng TiO2 oxy 6% vi cc thi gian phn x khc nhau.

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Hnh 4a. nh AFM ca mng TiO2 c nng oxy l 15% mp m Rms l 1,086 nm.

Hnh 4b. nh AFM ca mng TiO2 c nng oxy l 12% mp m Rms l 1,505 nm.

Hnh 4c. nh AFM ca mng TiO2 c nng oxy l 6% mp m Rms l 2,826 nm.

Ta nhn thy, mp m b mt Rms ca cc mng tng nh ( mn gim) v kch thc ht tng khi t l oxy gim t 15% xung 6% (hnh 4). Tuy vy, ta nhn thy cu trc ca chng hu nh l v nh hnh v mp m b mt Rms kh thp, thch hp cho vic ch to mng quang hc. Ngoi ra khi so snh cu trc mng t hnh 4a,4b v 4c, ta nhn thy nng 6% mng pht trin cu trc c trng ca tinh th TiO2 (ht hnh chp) v mt mng ln hn cc nng khc. gii thch hin tng ny, theo [4] l xut pht t bn cht ca qu trnh phn x kh phn ng. Nu t l oxy gia tng, ko theo s gia tng lp oxit bao ph b mt bia kim loi vi mi lin kt Ti-O, lm gia tng vic cch in. Do vy, th p vo gia tc cc ht ion v electron s b gim tc dng, cc ht phn x ra t bia khng nng lng pht trin tinh th trn . V nhng l do trn, mng c ch to vi nng oxy ln thng tn ti di dng v nh hnh. Ta c th theo di s thay i cu trc ca mng r hn na, nu ta to mng cng sut phn x cao t 200 250W. Tuy

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TP CH PHT TRIN KH&CN, TP 9, S 9 -2006

nhin, to mng v nh hnh c c tnh thch hp cho ng dng quang hc, nn trong bo co ny chng ti ch to mng cng sut l 90W. i vi mng SiO2 tuy c ch to bng phng php rf t bia gm SiO2, nhng trnh mt mt oxy trong hp thc mng chng ta cng cn phi b sung thm oxy trong qu trnh phn x. Theo [6], chit sut SiO2 t b nh hng bi nng oxy, nn trong bo co ny chng ti kho st ch to mng c nng oxy l 4% v 6%.
95 90 85

O TRUYEN QUA (%)

80 75 70 65 60 300 400 500 600 700 800 900 1000 1100 1200

B C S O N G ( n m )

Hnh 5. Ph truyn qua ca mng SiO2 c to nng oxy l 6% .

truyn qua ca mng trong vng kh kin kh cao khong 91%.

Hnh 6. nh chp AFM ca mng mng SiO2 trn thy tinh khng nung nhit, nng oxy l 4%.

mp m b mt ca mng rt thp, Rms khong 1,086 nm. Cu trc ca mng l hon ton v nh hnh.

Hnh 7. nh chp AFM ca mng mng SiO2 trn thy tinh khng nung nhit, nng oxy l 6%. Rms Rough: 0,3286 nm;

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S v nh hnh trong cu trc ca mng TiO2 v SiO2 li l mt thun li cho chng ta khi dng chng ch to mng a lp chng phn x AR. Do bi mng v nh hnh s c b mt phng hn v Rms thp hn rt nhiu so vi mng c cu trc tinh th (iu ny c chng ti trnh by trong cc bo co trc y), nn mng v nh hnh s c mt mt quang hc nh tn x rt thp. Ngoi ra, khi ch to mng a lp vi yu cu nghim ngt v chnh xc ca dy cc lp mng, th mng v nh hnh c b mt bng phng cng l mt li th rt ln.

Hnh 8. nh chp AFM i vi trn cha ph mng.

mp m ca b mt Rms ca thy tinh trn l 0,945 nm. Khi ta so snh Rms ca thy tinh trn vi Rms ca mng SiO2 (0,3286 nm) ta nhn thy Rms ca mng SiO2 hi thp hn ca trn, iu ny cho thy lc ban u lng ng trn , SiO2 lp y v lm phng nhng ch mp m b mt . T y ta c th kt lun l mp m ca b mt mng khng b nh hng bi . T nhng kho st cc c tnh quang v cu trc mng theo nng oxy, chng ti to mng chng phn x 2 lp (Double AR) vi nng oxy l 6%. ng thi vi chng trnh m phng tnh ton mng AR (chng ti trnh by cc bo trc y [7],[8]), chng ti chn b dy ca mi lp nh sau: TiO2 SiO2 khng kh l -15 nm 120 nm khng kh. Chit sut ti bc sng 500nm ca mng TiO2 khong 2.42, mng SiO2 l 1.46 v ca l 1.54. Kt qu ch to c trnh by hnh 9,
9 7 9 6 9 5

. . . . . . . . . e c h a p h u m a n g M a n g 2 l p A R

O TRUYEN QUA (%)

9 4 9 3 9 2 9 1 9 0 4 0 0 5 0 0 6 0 0 7 0 0 8 0 0

B C

S O N G

(n m )

Hnh 9. Ph truyn qua ca mng chng phn x 2 lp.

Hnh 9 cho ta thy mng 2 lp AR gia tng ng k truyn qua t khong 92% cho thy tinh trn cha ph mng ln n khong 96.4% (ti bc sng truyn qua cc i 500 nm). Vy chng ta gia tng truyn qua c khong 4.4%. Cng vi vic o hp thu ca thy tinh lam c l khong 2.2%, chng ta c th xc nh c phn x ca mng AR nh sau:

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TP CH PHT TRIN KH&CN, TP 9, S 9 -2006


. . . . . . . . . M o p h o n g D T h c n g h i e m
10

PHAN XA (%)

0 400 500 600 700 800

B C S O N G ( n m )

Hnh 10. Ph phn x ca mng 2 lp AR so snh gia m phng v thc nghim.

So snh ph phn x ca mng 2 lp AR gia m phng v thc nghim, ta thy chng c dng ging nhau, cng l dng V-shape v c nh ph bc sng 500 nm. Tuy nhin, phn x cc tiu ca mng thc nghim hi cao hn so vi mng m phng, mng thc nghim l 1.7% so vi mng m phng l 0%. Do nhng kh khn khch quan trong qu trnh to mng nh sau: 1. Sai s v dy gia cc lp mng, do h phn x ca chng ti khng c b phn o v khng ch dy trc tip trong qu tnh to mng. 2. Do s tn x ca , do l lam c khng phi l thy tinh thch anh quang hc vi cc thng s l tng nh trong chng trnh m phng. 3. Do s khng tinh khit ca mng TiO2, do mng chng ti to t target Ti c tinh khit l 98% - 99%, nn mng cng c hp thu nht nh trong vng kh kin. Tuy cn gp nhiu kh khn trong qu trnh to mng, nhng chng ti c bn to c mng chng phn x AR vi truyn qua c ci thin kh cao khong 4.5%. Cng vi chng trnh m phng mng, vic nghin cu mng a lp c rt nhiu thun li. Cc kt qu t c ny l c s chng ti nghin cu tip theo v mng AR vi cc kt qu tt hn.
4. KT LUN

Qua nghin cu ny, chng ta nhn thy mng TiO2 v SiO2 c ch to cng sut thp 90 W v nng oxy 6% c truyn qua cao, c chit sut v cu trc ph hp nht vi vic ch to mng chng phn x AR. Mng 2 lp AR gia tng ng k truyn qua t khong 92% cho trn cha ph mng ln n khong 96.4%. Kt qu ch to mng AR t c cn hn ch do nhiu nguyn nhn khch quan khi nghin cu. Tuy nhin, t cc kt qu t c trn, s l c s cho chng ti tip tc ci tin nng cao cht lng ca mng chng phn x 2 lp, cng nh m rng ch to mng 3-4 lp sau ny.

STUDYING OPTIMAL PARAMETERS OF TiO2 AND SiO2 THIN FILMS TO PREPARE FOR ANTI-REFLECTION COATING
Le Vu Tuan Hung, Nguyen Van Den, Huynh Thanh Dat University of Natural Siences, VNU-HCM ABSTRACT: TiO2 thin film was fabricated by dc sputtering, SiO2 was made by rf sputtering with various ratio of O2 / Ar+O2 = 30%, 15%, 12% and 6%. The optical

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characteristics of films were determined by transmittance spectra UV-Vis. The structure and roughness surface Rms were investigated by AFM method. The ratio of O2 of 6% is the best condition to prepare for anti-reflection coating (AR) double layers. It can increase about 4.5 % the transmittance if comparing with bare substrate.

TI LIU THAM KHO

[1]. C.Martinet, Deposition of SiO2 and TiO2 thin films by plasma enhanced chemical vapor deposition for antireflection coating, Journal of Non- Crystalline Solids 216 77-82.,(1997). [2]. Andrew Soutar, Bart Fokkink, Sol-gel anti-reflective coatings, SIMTech Technical Report (PT/01/002/ST). [3]. T. Takahashi, Dependence of working gas pressure and ratio of Ar to O2 on properties of TiO2 films deposited by facing targets sputtering, Thin Solid Films 420-421 433-437., (2002). [4]. K.G.Geraghty and L.D.Donaghey, Preparation of suboxides in the Ti-O system by reactive sputtering, Thin Solid Films, 40 375-383., (1977). [5]. Hans Bach, Dieter Krause, Thin film on glass, 137-205.,(1997). [6]. Sang- Hun Jeong, Characterization of SiO2 and TiO2 films prepared using rf magnetron sputtering and their application to anti-reflection coating,Vacuum 76, 507-515., (2004). [7]. L V Tun Hng, Nguyn Vn n, Tnh ton dy ti u cho cc lp mng a lp in mi chng phn x trong vng hng ngai bng phng php N-Squared Scan, Tp ch Pht trin KH&CN V.7, 4&5/2004. [8]. L V Tun Hng, Nguyn Vn n, Xc nh t hp ti u cho mng chng phn x a lp bng phng php Flip-Flop, Tp ch Pht trin KH&CN V.7, 6/2004.

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