Chế tạo màng tio2ag và tio2au bằng phương pháp bốc bay laser và ứng dụng tính chất quang xúc tác của màng để xử lí hợp chất hữu cơ khó phân huỷ trong nước

LI CAM OAN Tụi xin cam oan bn lun ny l kt qu nghiờn cu ca cỏ nhõn tụi Cỏc s liu v ti liu c trớch dn lun l trung thc Kt qu nghiờn cu ny khụng trựng vi bt c cụng trỡnh no ó c cụng b trc ú Tụi chu trỏch nhim vi li cam oan ca mỡnh H Ni, 01 thỏng 06 nm 2017 Tỏc gi lun Nguyn Tin Hng LI CM N u tiờn, cho phộp em c gi li cm n chõn thnh v sõu sc ti TS Nguyn Tin Dng, ngi thy ó tn tỡnh ch bo em cng nh to mi iu kin thun li em cú th trung lm lun Em xin trõn trng cm n TS Nguyn Cao Khang, ngi thy ó nhit tỡnh ch bo em, giỳp v khớch l em rt nhiu sut thi gian em lm lun Em xin chõn thnh cm n ton th thy cụ giỏo khoa Húa hc núi chung v cỏc thy cụ t Mụi trng núi riờng ó trang b kin thc, chia s kinh nghim, ng viờn, giỳp em sut thi gian em hc Em xin gi li cm n ti cỏc anh ch nghiờn cu sinh, cỏc anh ch cao hc cựng cỏc bn sinh viờn lm vic ti Trung tõm Khoa hc v Cụng ngh Nano Trng i hc S phm H Ni, nhng ngi ó luụn giỳp , chia s kinh nghim cho em sut thi gian em lm vic ti trung tõm Cui cựng, xin by t tỡnh cm ti gia ỡnh, nhng ngi thõn v bn bố ó luụn yờu thng, ng viờn, chia s v giỳp em em cú th trung hon thnh lun H Ni, ngy thỏng nm 2017 Nguyn Tin Hng MC LC M U CHNG 1: TNG QUAN 1.1 Cu trỳc tinh th TiO2 1.2 Mt s tớnh cht vt lý v húa hc ca TiO2 1.2.1 Tớnh cht vt lý 1.2.2 Tớnh cht húa hc 11 1.3 Tng quan v mng TiO2 12 1.4 Tớnh cht quang xỳc tỏc ca TiO2 13 1.4.1 C ch quang xỳc tỏc ca TiO2 13 1.4.2 Cỏc bin phỏp nõng cao hiu qu xỳc tỏc quang húa ca TiO2 17 1.5 ng dng ca TiO2 21 1.5.1 Phõn loi mt s ng dng ca TiO2 da theo tớnh cht ca nú 21 1.5.2 ng dng vic x lớ cỏc cht ụ nhim mụi trng 23 1.6 Tng quan v vt liu vng (Au) 23 1.6.1 Cu trỳc tinh th vng Au 23 1.6.2 Cỏc tớnh cht ca Au 24 1.6.3 Tng quan v ht nano vng 25 1.7 Tng quan v vt liu bc (Ag) 26 1.7.1 Cu trỳc tinh th bc (Ag) 26 1.7.2 Cỏc tớnh cht ca Ag 27 1.7.3 Tng quan v ht nano bc 28 1.8 Tỡm hiu v vt liu TiO2/Ag v TiO2/Au 28 CHNG THC NGHIM CH TO MU 30 2.1 Cỏc phng phỏp ch to vt liu 30 2.1.1 To mng TiO2 bng phng phỏp spin coating 30 2.1.2 Ph Au, Ag lờn mng TiO2 bng phng phỏp bc bay laser xung (PLD) 35 2.2 Cỏc phng phỏp kho sỏt cu trỳc v hỡnh thỏi b mt vt liu 38 2.2.1 Phng phỏp nhiu x tia X 38 2.2.2 Phộp o ph tỏn x Raman 40 2.2.3 Phng phỏp kớnh hin vi in t quột (SEM) 42 2.3 Cỏc phng phỏp kho sỏt tớnh cht quang ca vt liu 43 2.3.1 Phộp o ph hp th 43 2.3.2 Phộp o ph hunh quang 47 2.4 Phng phỏp nghiờn cu xỳc tỏc quang phõn hy xanh methylene (MB) 49 2.5 Nghiờn cu kh nng x lớ nc thi dt nhum 50 CHNG 3: KT QU V THO LUN 53 3.1 Hỡnh thỏi b mt 54 3.2 Cu trỳc vt liu 56 3.2.1 Kt qu phõn tớch cu trỳc t ph nhiu x tia X 56 3.2.2 Kt qu phõn tớch cu trỳc t ph tỏn x Raman 59 3.3 Tớnh cht quang 61 3.3.1.Ph hp th 61 3.3.2 Ph hunh quang 64 3.4.2 Xõy dng ng chun xỏc nh nng MB theo cng hp th 70 3.4.3 Kt qu quang xỳc tỏc ca vt liu di ỏnh sỏng nhỡn thy 71 3.4.4 Kt qu quang xỳc tỏc ca vt liu di ỏnh sỏng mt tri: 73 3.5 X lớ vi mu nc thi dt nhum 74 3.5.1 Xõy dng ng chun xỏc nh hm lng COD 74 3.5.2 Kt qu kho sỏt kh nng x lớ mu nc thi dt nhum 76 KT LUN CHUNG 79 TI LIU THAM KHO 81 DANH MC BNG Bng 1.1 Thụng s vt lý ca TiO2 pha anasate v rutile Bng 1.2 Bng mt s ng dng ca TiO2 [10,13] 21 Bng 3.1 Kớ hiu cỏc mu mng c ch to khúa lun 53 Bng 3.2 Cng hp th ca MB 70 Bng 3.3 Bng th tớch cỏc dung dch xõy dng ng chun COD 75 Bng 3.4 Giỏ tr COD ca mu nc thi (mu pha loóng ln, x lớ 6h) 77 Bng 3.5 Giỏ tr COD ca mu nc thi (mu pha loóng 10 ln, x lớ 12h) 77 DANH MC HèNH Hỡnh 1.1 Cỏc dng thự hỡnh khỏc ca TiO2: (A) rutile, (B) anatase, (C) brookite Hỡnh 1.2 Khi bỏt din ca TiO2 Hỡnh 1.3 Cu trỳc tinh th ca TiO2: (A) rutile, (B) anatase Hỡnh 1.4 Cu trỳc tinh th ca TiO2 brookite Hỡnh 1.5 Ph hp th ca tinh th TiO2 hon ho theo bc súng [35] 10 Hỡnh 1.6 Ph hp th ca tinh th TiO2 hon ho theo nng lng [35] 10 Hỡnh 1.7 Cu trỳc vựng nng lng ca cht bỏn dn v s hot ng ca cht bỏn dn c kớch thớch quang hoỏ 14 Hỡnh 1.8 C ch phn ng quang xỳc tỏc ca TiO2 c chiu sỏng bi bc súng thớch hp 14 Hỡnh 1.9 Cu trỳc lp phng tõm mt tinh th Au 24 Hỡnh 1.10 Hin tng cng hng plasmon b mt 25 Hỡnh 1.11 Cu trỳc tinh th ca bc 27 Hỡnh 2.1 Cỏc giai on ca phng phỏp ph quay 30 Hỡnh 2.2 S túm tt quy trỡnh ch to sol TiO2 33 Hỡnh 2.3 S túm tt quy trỡnh ph mng nano TiO2 34 Hỡnh 2.4 S nguyờn lý to mng dựng tia laser 35 Hỡnh 2.5 Hin tng nhiu x xy trờn mt h mt phng mng tinh th 38 Hỡnh 2.6 S nguyờn lý tỏn x Raman 41 Hỡnh S nguyờn lý kớnh hin vi in t quột 43 Hỡnh 2.8 S hp th ỏnh sỏng qua mu 44 Hỡnh 2.9 Nguyờn tc o hp th bng qu cu tớch phõn: 46 Hỡnh 2.10 S ca h o hunh quang 48 Hỡnh 2.11 H quang xỳc tỏc phõn hy MB 49 Hỡnh 3.1 S túm tt quy trỡnh ch to cỏc mu 53 Hỡnh 3.2 nh SEM b mt v b dy mng TiO2 [10] 54 Hỡnh 3.3 nh SEM ca mu TiO2/Ag 55 Hỡnh 3.4 nh SEM ca mu TiO2/Au 55 Hỡnh 3.5 Gin nhiu x tia X ca mu TiO2/Ag (a) v mu TiO2/Au (b) 57 Hỡnh 3.6 Ph Raman ca cỏc mu TiO2/Ag (a) v cỏc mu TiO2/Au (b) 60 Hỡnh 3.7 Ph hp th ca cỏc mu mng TiO2/Ag (a) v TiO2/Au (b) 61 Hỡnh 3.8 Ph hp th in hỡnh ca ht nano vng 63 Hỡnh 3.9 Ph hp th in hỡnh ca ht nano bc 63 Hỡnh 3.10 Kt qu o ph hunh quang ca cỏc mu (Ag/TiO2)1-3 65 Hỡnh 3.11 Kt qu o ph hunh quang ca cỏc mu (Au/TiO2)1-3 66 Hỡnh 3.12 Cu to ca MB C16H18N3SCl 69 Hỡnh 3.13 ng chun xỏc nh mng MB 71 Hỡnh 3.14 S suy gim nng MB theo thi gian s dng cỏc mu mng TiO2/Ag (a) v TiO2/Au (b) (ỏnh sỏng ốn dõy túc) 72 Hỡnh 3.15 S suy gim nng MB theo thi gian s dng cỏc mu mng TiO2/Ag (a) v TiO2/Au (b) (ỏnh sỏng mt tri) 74 Hỡnh 3.16 ng chun xỏc nh COD 76 DANH MC Kí HIU V CH VIT TT SPR : Surface Plasmon Resonance (hin tng cng hng plasmon b mt) PLD : Plasma Laser Deposition (phng phỏp ph mng bng xung laser) COD : Chemical Oxygen Demand (nhu cu oxy húa hc) SEM : Scanning Electron Microscope (kớnh hin vi in t quột) TTIP UV-Vis XRD PL : Titanium tetraisoproproxide : Bc x t ngoi - Kh kin : X-ray Diffraction (nhiu x tia X) : Photoluminescence (ph quang phỏt quang) : Bc súng ỏnh sỏng : Gúc nhiu x tia X MB : Metylenne Blue (xanh metylen) M U Ngy nay, ụ nhim mụi trng, c bit l ụ nhim ngun nc ó v ang ngy cng tr nờn nghiờm trng Vit Nam Trờn cỏc phng tin truyn thụng, chỳng ta cú th d dng bt gp nhng hỡnh nh, nhng thụng tin mụi trng b ụ nhim Bt chp nhng li kờu gi bo v mụi trng, bo v ngun nc, tỡnh trng ụ nhim cng lỳc cng tr nờn trm trng Cú nhiu nguyờn nhõn khỏch quan v ch quan dn n tỡnh trng ny nh: s gia tng dõn s, quỏ trỡnh cụng nghip hoỏ, hin i hoỏ, c s h tng yu kộm, lc hu, nhn thc ca ngi dõn v mụi trng cũn cha cao Hu qu chung ca tỡnh trng ụ nhim ngun nc l mụi trng sng b nh hng, t l ngi mc cỏc bnh cp v mn tớnh liờn quan n ụ nhim nh viờm mng kt, tiờu chy, ung th ngy cng tng ng trc tỡnh trng ny, vic x lý cỏc cht ụ nhim bng nhng cht xỳc tỏc thõn thin vi mụi trng thay th cỏc quỏ trỡnh x lý cú hiu sut thp v thi nhiu cht c hi ó v ang c quan tõm Nm 1972, Fujishima v Honda ó khỏm phỏ tỏc dng quang xỳc tỏc ca TiO2 phõn tỏch nc thnh Hydro v Oxy di tỏc dng ca tia t ngoi [27] T ú tỏc dng quang xỳc tỏc ca TiO2 ó c chỳ ý bi kh nng tim tng ca nú vic chuyn i nng lng ỏnh sỏng thnh nng lng húa hc c bit, hin TiO2 cũn c s dng nh mt cht xỳc tỏc quang húa bi s thõn thin vi mụi trng v kh nng vt tri vic x lý cỏc cht ụ nhim nh cỏc cht hu c, vi khun, vi rỳt, khụng khớ v nc [40,46] Tuy nhiờn TiO2 ch hp th ỏnh sỏng vựng t ngoi Qua thng kờ, ỏnh sỏng vựng t ngoi ch chim 5% ỏnh sỏng mt tri [27] Nu dựng tinh khit Mng TiO2 ph Ag cú kh nng phõn hy MB tt hn mng TiO2 ph Au Mu ln ph cú hiu sut quang xỳc tỏc ln nht ri n mu ln ph, cui cựng l mu ln ph Kt qu ny cng phự hp vi kt qu ph hunh quang ca cỏc mu Mu TiO2/Ag cú kh nng phõn hy MB tt nht (80%), mu (TiO2/Au)2 cú kh nng phõn hy MB kộm nht (48%) Hiu sut ca phn ng quang xỳc tỏc ca cỏc mu ph thuc vo nhiu yu t, ú phi k n vai trũ c bn l s tỏch cp e h Cỏc cp e h ny di chuyn n b mt to cỏc gc t cú kh nng oxi húa mnh Hiu sut quang xỳc tỏc khụng tng dn t mu ln ph n mu ln ph cú th c gii thớch lp kim loi ngoi cựng (lp tip xỳc trc tip vi MB) Kớch thc v khong cỏch gia cỏc ht Ag, Au lp ngoi cựng s nh hng n kh nng quang xỳc tỏc ca mng Cỏc mu mng ph Ag cú kt tinh tt, kớch thc v khong cỏch cỏc ht ng u l nhng yu t quan trng lm gim s tỏi hp cỏc cp e h [17,53,56] iu ú dn n hiu sut cng nh tc ca phn ng quang xỳc tỏc phõn hy MB ca cỏc mu ph Ag l tt hn 3.4.4 Kt qu quang xỳc tỏc ca vt liu di ỏnh sỏng mt tri Cỏc mu mng tip tc c kho sỏt kh nng quang xỳc tỏc phõn hu dung dch xanh metylen di ỏnh sỏng mt tri 73 Hỡnh 3.15 S suy gim nng MB theo thi gian s dng cỏc mu mng TiO2/Ag (a) v TiO2/Au (b) (ỏnh sỏng mt tri) Kt qu cho thy vi iu kin chiu ỏnh sỏng mt tri thỡ kh nng quang xỳc tỏc ca vt liu tt hn s dng búng ốn si t C th, hiu sut phõn hu MB cao nht di ỏnh sỏng Mt tri l 86%, ln hn so vi trng hp dựng ngun sỏng l búng ốn si t (80%); hiu sut phõn hu MB thp nht di ỏnh sỏng mt tri l 53%, ln hn so vi trng hp dựng ngun sỏng l búng ốn si t (48%) Hiu sut tng dựng ỏnh sỏng Mt tri cú th hai nguyờn nhõn chớnh: (1) cng sỏng ca Mt tri 20400 lux ln hn cng sỏng ca ốn si t 11200 lux, (2) ỏnh sỏng Mt tri cú mt phn tia UV Nh vy, vt liu hon ton cú kh nng ng dng vo thc t vic x lý cỏc cht hu c 3.5 X lớ vi mu nc thi dt nhum 3.5.1 Xõy dng ng chun xỏc nh hm lng COD - S dng ng phỏ mu COD ỏnh s th t t 1-7 - Chun b dung dch vi th tớch cỏc cht nh bng 3.3 74 Bng 3.3 Bng th tớch cỏc dung dch xõy dng ng chun COD STT COD (mg/l) KHP (ml) H2O (ml) K2Cr2O7 (ml) Ag2SO4 (ml) 0 2,500 1,500 3,500 50 0,125 2,375 1,500 3,500 100 0,250 2,250 1,500 3,500 200 0,500 2,000 1,500 3,500 400 1,000 1,500 1,500 3,500 600 1,500 1,000 1,500 3,500 900 2,250 0,250 1,500 3,500 y np ng phỏ mu v lc u t ng phỏ mu ny vo mỏy phỏ mu COD (HACH) vi nhit 150oC 120 phỳt, sau ú ngui ri em i o cỏc giỏ tr mt quang Kt qu thu c nh sau: Bng Giỏ tr COD vi mt quang tng ng STT COD (mg/l) Abs 0,020 50 0,037 100 0,059 200 0,095 400 0,145 600 0,219 900 0,312 75 0.35 y = 0,00032x + 0,02340 R = 0,998 0.3 0.25 0.2 0.15 0.1 0.05 0 200 400 600 800 1000 Hỡnh 3.16 ng chun xỏc nh COD Tin hnh x lớ thng kờ theo phng phỏp bỡnh phng ti thiu biu din s ph thuc mt quang vo COD tng ng v ta thu c phng trỡnh ng chun dng Abs = aCOD + b nh sau: Abs = 0,00032ìCOD + 0,02340 3.5.2 Kt qu kho sỏt kh nng x lớ mu nc thi dt nhum Mu nc thi dt nhum c ly ti lng Vn Phỳc, H ụng, H Ni Mu c pha loóng ln v 10 ln Giỏ tr COD ca mu nc c xỏc nh trc v sau tin hnh x lớ nh sỏng c s dng kớch thớch phn ng quang xỳc tỏc l ỏnh sỏng ốn dõy túc 200W 220V Bc súng m ốn phỏt ch yu nm vựng bc x kh kin v hng ngoi Kh nng quang xỳc tỏc ca cỏc mu c ỏnh giỏ thụng qua vic xỏc nh giỏ tr COD ca nc thi sau x lớ 76 Bng 3.5 Giỏ tr COD ca mu nc thi (mu pha loóng ln, x lớ 6h) CODu Mu mng TiO2/Ag 131,25 54,84 (TiO2/Ag)2 168,75 41,81 (TiO2/Ag)3 156,25 46,24 TiO2/Au 143,75 50,54 (TiO2/Au)2 171,87 40,86 (TiO2/Au)3 161,28 44,39 290,00 CODcui Hiu sut STT (%) Trờn bng 3.4 cho thy mng TiO2 ph Ag cú kh nng x lớ tt hn mng TiO2 ph Au Mu ln ph cú hiu sut quang xỳc tỏc ln nht ri n mu ln ph, cui cựng l mu ln ph Tuy nhiờn mu (TiO2/Au)3 li cú hiu sut x lớ nc thi tt hn so vi mu (TiO2/Ag)2 iu ny cú th thnh phn cỏc hoỏ cht nc thi lm nh hng n hiu sut x lớ nc thi ca mu mng Mu TiO2/Ag cú kh nng x lớ nc thi tt nht (54,80%), mu (TiO2/Au)2 cú kh nng x lớ kộm nht (40,86%) Bng 3.6 Giỏ tr COD ca mu nc thi (mu pha loóng 10 ln, x lớ 12h) STT Mu mng TiO2/Ag (TiO2/Ag)2 (TiO2/Ag)3 CODu 118,75 77 CODcui Hiu sut (%) 55,12 53,58 62,50 47,36 57,75 51,37 TiO2/Au 62,50 47,36 (TiO2/Au)2 81,25 31,57 (TiO2/Au)3 76,87 35,27 Khi pha loóng hn v tng kh nng x lớ thỡ ch cú mu TiO2/Ag v (TiO2/Ag)3 cú kh nng x lớ lm giỏ tr COD gim xung gn giỏ tr 50 nht Cỏc mu ln ph cho thy hiu sut quang xỳc tỏc tt hn so vi mu v ln ph Nhng nghiờn cu bc u ny m trin vng ỏp dng mng TiO2/Ag v TiO2/Au n lp v a lp x lớ nhiu ngun nc thi cú cha cỏc hp cht hu c l rt ln, gúp phn vo nhim v x lớ ụ nhim mụi trng ang c t cp bỏch hin 78 KT LUN CHUNG T nhng kt qu nghiờn cu chỳng tụi thu c mt s kt lun sau õy: Ch to thnh cụng mng mng TiO2/Ag v TiO2/Au vi s lp mng khỏc bng phng phỏp spin coating v phng phỏp bc bay laser Cỏc mu mng ch to c cú cu trỳc tinh th TiO2 pha anasate v rutile Trong iu kin sol ch to cú nng 0,1 M, pH = 1, nhit nung l 400oC thi gian gi thỡ s phõn ró ca cỏc ht bc tt hn so vi cỏc ht vng Cỏc ht bc c to thnh cú kớch thc tng i ng u, khong cỏch gia cỏc ht cng u hn so vi cỏc ht vng Kớch thc v khong cỏch ca cỏc ht nano bc v vng c to thnh cú nh hng trc tip ti kh nng quang xỳc tỏc ca cỏc mu mng Cỏc mu mng TiO2/Ag v TiO2/Au vi cỏc lp khỏc ó ch to c ngoi nhng bc x vựng t ngoi cũn hp th tt cỏc bc x cú bc súng t 400 n 800 nm Trong ú, cng hp th ca mu lp l cao nht, sau ú n mu lp v cui cựng l mu lp iu ny chng t hin tng cng hng plasmon b mt cỏc ht kim loi bc v vng kớch thc nano gõy ó lm tng kh nng hp th ca cỏc mu mng vựng ỏnh sỏng nhỡn thy Kt qu kho sỏt tớnh quang xỳc tỏc vic phõn hy hp cht xanh metylen ca cỏc mu ch to cho thy cỏc mu mng TiO2 ph Ag v Au u cú kh nng phõn hy xanh metylen vựng ỏnh sỏng nhỡn thy tt hn so vi TiO2 tinh khit Sau gi chiu sỏng, mu TiO2/Ag cho kh nng phõn hy cao nht phõn hy c 80% (vi ỏnh sỏng ốn si t) v 84% (vi ỏnh sỏng mt tri) dung dch xanh metylen, mu (TiO2/Au)2 phõn hy thp nht c 48% (vi ỏnh sỏng ốn si t) v 79 53% (vi ỏnh sỏng mt tri) dung dch xanh metylen Kh nng quang xỳc tỏc phõn hy MB ca cỏc mu khụng ph thuc tuyn tớnh theo hm lng Ag, Au S dng mu mng x lớ nc thi dt nhum ca lng Vn Phỳc, H ụng, H Ni cho thy cỏc mu mng TiO2 ph Ag v Au u cú kh nng x lớ nc thi Sau 6h chiu sỏng liờn tc, mu TiO2/Ag cho thy hiu sut x lớ cao nht (54,84%), giỏ tr COD gim t 290 xung cũn 131,25 80 TI LIU THAM KHO o Khc An (Ch biờn) (2012), Mt s phng phỏp vt lớ thc nghim hin i, NXB Giỏo dc Vit Nam, H Ni Ngc An Bang, Lờ Vn V (2007), Ch to v nghiờn cu mt s tớnh cht quang ca ht vng (Au) cú kớch thc nano, Hi ngh Vt lý cht rn ton quc ln th V, 773 - 776 B Ti nguyờn v mụi trng, Quy chun k thut quc gia v nc thi cụng nghip dt nhum, QCVN 13 - MT:2015/BTNMT B Ti nguyờn v mụi trng, Cht lng nc - Xỏc nh nhu cu oxy hoỏ hc (COD), TCVN 6491:1999 (ISO 6060:1989) V ỡnh C, Nguyn Xuõn Chỏnh (2004), Cụng ngh nano iu khin n tng phõn t, nguyờn t, NXB Khoa hc v k thut, H Ni Lờ Cụng Dng (2000), Vt liu hc, NXB Khoa hc k thut, H Ni Trn Thu H (2011), Hin tng cng hng plasmon b mt ca cỏc ht nano kim 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Chế tạo màng TiO2/Ag TiO2/Au phương pháp bốc bay laser ứng dụng tính chất quang xúc tác màng để xử lí hợp chất hữu khó phân huỷ nước Mục đích nghiên cứu luận văn: - Chế tạo màng mỏng TiO2 phương. .. nghiệm: Trình bày phương pháp chế tạo màng mỏng TiO2/Ag TiO2/Au; phép đo thực để khảo sát hình dạng cấu trúc, tính chất quang, khả quang xúc tác mẫu chế tạo, khả xử lí nước thải thực tế màng ✓ Chương... Tính chất quang xúc tác TiO2 Chất xúc tác chất có tác dụng làm giảm lượng kích hoạt phản ứng hóa học không bị sau phản ứng Nếu trình xúc tác kích thích ánh sáng gọi quang xúc tác Chất có tính hoạt