I HC QUC GIA H NI TRNG I HC KHOA HC T NHIấN NGễ QUANG BINH NGHIấN CU TNG HP, C TRNG V KH NNG HP PH ASEN CA VT LIU TRấN C S CACBON (GRAPHEN OXIT, GRAPHEN) CHUYấN NGNH: HểA Vễ C M S: 60440113 LUN VN THC S KHOA HC NGI HNG DN KHOA HC TS V èNH NG H Ni - Nm 2015 MC LC LI CM N i LI CAM OAN ii DANH MC CC T VIT TT iii DANH MC CC BNG BIU iv DANH MC CC HèNH V v M U Error! Bookmark not defined CHNG 1: TNG QUAN Error! Bookmark not defined 1.1 Gii thiu v vt liu Cacbon Error! Bookmark not defined 1.1.1 Kim Cng Error! Bookmark not defined 1.1.2 Graphit Error! Bookmark not defined 1.1.3 Fulleren Error! Bookmark not defined 1.1.4 ng nano cacbon Error! Bookmark not defined 1.1.5 Graphen Error! Bookmark not defined 1.2 Tng quan v graphen Error! Bookmark not defined 1.2.1 Phõn loi graphen Error! Bookmark not defined 1.2.2 Tớnh cht ca graphen Error! Bookmark not defined 1.2.3 Cỏc phng phỏp tng hp graphen Error! Bookmark not defined 1.2.3.1 Phng phỏp tỏch lp vi c hc Error! Bookmark not defined 1.2.3.2 Phng phỏp epitaxy Error! Bookmark not defined 1.2.3.3 Phng phỏp húa hc Error! Bookmark not defined 1.2.4 ng dng ca graphen Error! Bookmark not defined 1.3 Graphen Oxit (GO) Error! Bookmark not defined 1.4 Vt liu composit gia Graphen oxit, Graphen vi Fe3O4 Error! Bookmark not defined 1.5 Tng quan v Asen v phng phỏp x lý Asen Error! Bookmark not defined 1.5.1 Gii thiu v Asen Error! Bookmark not defined Ngụ Quang Binh a Lun thc s 1.5.2 Mt s phng phỏp x lý ụ nhim asen Error! Bookmark not defined 1.5.2.1 Phng phỏp kt ta, lng/lc Error! Bookmark not defined 1.5.2.2 Phng phỏp hp ph v trao i ion Error! Bookmark not defined 1.5.2.3 Cỏc phng phỏp vt lý Error! Bookmark not defined 1.5.2.4 Phng phỏp s dng thc vt (phytoremediation) Error! Bookmark not defined 1.6 Lý thuyt v hp ph Error! Bookmark not defined 1.6.1 Hin tng hp ph Error! Bookmark not defined 1.6.2 Phõn loi cỏc dng hp ph Error! Bookmark not defined 1.6.2.1 Hp ph vt lý Error! Bookmark not defined 1.6.2.2 Hp ph hoỏ hc Error! Bookmark not defined 1.6.3 S hp ph mụi trng nc Error! Bookmark not defined 1.6.4 Mt s mụ hỡnh ng nhit hp ph Error! Bookmark not defined CHNG 2: CC PHNG PHP NGHIấN CU V THC NGHIM Error! Bookmark not defined 2.1 Húa cht Error! Bookmark not defined 2.2 Thc nghim Error! Bookmark not defined 2.2.1 Tng hp graphit oxit t graphit Error! Bookmark not defined 2.2.2 Tng hp graphen oxit (GO) Error! Bookmark not defined 2.2.2.1 Phng phỏp c hc (siờu õm) Error! Bookmark not defined 2.2.2.3 Phng phỏp vi súng Error! Bookmark not defined 2.2.3 Tng hp graphen Error! Bookmark not defined 2.2.3.1 Tng hp graphen bng phng phỏp kh húa hc Error! Bookmark not defined 2.2.3.2 Tng hp graphen bng phng phỏp kh nhit Error! Bookmark not defined 2.2.4 Tng hp ht nano composit Fe3O4 GO Error! Bookmark not defined Ngụ Quang Binh b Lun thc s 2.2.5 Chun b dung dch As(V) Error! Bookmark not defined 2.2.6 Thớ nghim hp ph As(V) Error! Bookmark not defined 2.3 Cỏc phng phỏp nghiờn cu Error! Bookmark not defined 2.3.1 Phng phỏp ph nhiu x tia X (XRD) Error! Bookmark not defined 2.3.2 Ph tỏn x tia X (EDX) Error! Bookmark not defined 2.3.3 Phng phỏp quang ph hng ngoi (IR) Error! Bookmark not defined 2.3.4 Phng phỏp hin vi in t quột (SEM) Error! Bookmark not defined 2.3.5 Phng phỏp hin vi truyn in t phõn gii cao (HR TEM) Error! Bookmark not defined 2.3.6 Phng phỏp ng nhit hp ph- kh hp ph N2 (BET) Error! Bookmark not defined 2.3.7 Phng phỏp hp ph nguyờn t (AAS) Error! Bookmark not defined CHNG 3: KT QU V THO LUN Error! Bookmark not defined 3.1 Kho sỏt nh hng cỏc yu t n quỏ trỡnh tng hp GO v Graphen (G) Error! Bookmark not defined 3.1.1 Kho sỏt nh hng ca nguyờn liu u Error! Bookmark not defined 3.1.2 Kho sỏt nh hng ca t l KMnO4/ Graphit Error! Bookmark not defined 3.1.3 Kho sỏt nh hng nhit Error! Bookmark not defined 3.1.4 Cỏc yu t nh hng n quỏ trỡnh búc lp GO bng k thut vi súng Error! Bookmark not defined 3.1.5 nh hng nhit n quỏ trỡnh kh GO v G Error! Bookmark not defined 3.2 c trng hỡnh thỏi hc ca vt liu GO v G kh nhit Error! Bookmark not defined Ngụ Quang Binh c Lun thc s 3.2.1 Phng phỏp nhiu x tia X (XRD) Error! Bookmark not defined 3.2.2 Ph hng ngoi chuyn dch Fourier (FTIR) Error! Bookmark not defined 3.2.3 Kớnh hin vi in t truyn qua phõn gii cao (HR TEM) Error! Bookmark not defined 3.2.4 Hp ph v kh hp ph Nit (BET) Error! Bookmark not defined 3.2.5 Quang ph XPS Error! Bookmark not defined 3.3 Kh nng hp ph asen ca GO, G, GO/Fe3O4 Error! Bookmark not defined 3.3.1 nh hng ca PH Error! Bookmark not defined 3.3.2 Nghiờn cu ng nhit hp ph Error! Bookmark not defined CHNG 4: KT LUN V KIN NGH Error! Bookmark not defined TI LIU THAM KHO PH LC Error! Bookmark not defined Ngụ Quang Binh d Lun thc s LI CM N hon thin lun ny ú l mt s n lc ln i vi tụi v tụi khụng th hon thnh nu khụng cú s giỳp quan trng ca rt nhiu ngi u tiờn tụi xin gi li cm n chõn thnh n thy TS V ỡnh Ng l ngi ó hng dn tn tỡnh cho tụi sut thi gian thc hin lun ny Thy ó cung cp cho tụi rt nhiu hiu bit v mt lnh vc mi tụi bt u bc vo thc hin lun Trong quỏ trỡnh thc hin lun thy luụn nh hng, gúp ý v sa cha giỳp tụi hon thnh tt lun ny Tụi xin chõn thnh cm n PGS.TS V Anh Tun, PGS.TS ng Tuyt Phng, TS Trn Th Kim Hoa cựng ton th anh ch ti phũng Hoỏ lý b mtVin Hoỏ hc-Vin Hn Lõm Khoa Hc v Cụng Ngh Vit Nam ó to mi iu kin giỳp tụi sut quỏ trỡnh thc hin lun ny Nhng li cm n sau cựng xin dnh cho cha m, v con, nhng ngi luụn bờn cnh chia s, bo ban cng nh ng viờn tụi sut thi gian qua, v tụi cng mun gi li cm n n nhng ngi thõn ó ht lũng quan tõm v to iu kin tt nht tụi hon thnh lun ny H Nụi, thỏng 01 nm 2015 HC VIấN THC HIN Ngụ Quang Binh Ngụ Quang Binh i Lun thc s LI CAM OAN Tụi xin cam oan õy l cụng trỡnh nghiờn cu ca riờng tụi, cỏc s liu v kt qu c a lun l trung thc, c cỏc ng gi cho phộp s dng v cha tng c cụng b bt k cụng trỡnh no khỏc Tỏc gi Ngụ Quang Binh Ngụ Quang Binh ii Lun thc s DANH MC CC T VIT TT AAS: Atomic Absorption Spectrophotometric (phng phỏp ph hp th nguyờn t ) BET: Brunauer-Emmett-Teller (Hp ph v kh hp ph Nit) EDX: Energy-dispersive X-ray spectroscopy (Phi tỏn x nng lng tia X) FTIR: Fourier transform infrared spectroscopy (Ph hng ngoi chuyn dch Fourier) G: Graphen GO: Graphen oxit GOVS: Graphen oxit tng hp theo phng phỏp vi súng GOSA: Graphen oxit tng hp theo phng phỏp siờu õm GO VS/ Fe3O4: Nanocomposit GO vi súng gn Fe3O4 GO kh nhit/ Fe3O4: Graphen oxit em kh nhit thnh Graphen, sau ú chc húa Fe3O4 GO kh N2H4/ Fe3O4: Graphen oxit em kh bng N2H4 thnh Graphen, sau ú chc húa Fe3O4 HR-TEM: High-resolution Transmission Electron Microscopy (Hin vi in t truyn qua phõn gii cao) pHpzc (pH The point of zero charge (pzc)): l giỏ tr pH m ti ú mt in tớch trờn b mt bng khụng UV-Vis: Ultravioletvisible spectroscopy (Ph t ngoi kh kin) XPS: X-ray photoelectron spectroscopy (Ph quang in t tia X) XRD: X-Ray diffraction (Nhiu x tia X) Ngụ Quang Binh iii Lun thc s DANH MC CC BNG BIU Bng 1.1 Tớnh cht ca ng nano cacbon Bng 1.2 Tớnh cht vt lý ca n lp graphen nhit phũng Bng 1.3 So sỏnh c tớnh gia thộp v cỏc vt liu carbon 11 Bng 1.4 ỏnh giỏ so sỏnh kh nng hp ph ca mt s vt liu khỏc x lý asen 28 Bng 3.1 Kho sỏt nh hng lng nguyờn liu ban u 54 Bng 3.2 Kho sỏt nh hng ca thi gian vi súng 54 Bng 3.3 Kho sỏt ch vi súng thớch hp 55 Bng 3.4 Cỏc thụng s c trng ca graphen oxit (a) v graphen (b) 62 Bng 3.5 Phn trm cỏc nguyờn t ph XPS ca GOSA v graphen 64 Bng 3.6 Kh nng hp ph As(V) ca GO siờu õm 65 Bng 3.7 S liu kh nng hp ph As(V) cỏc pH khỏc ca GOVS/Fe3O4 v GOVS 66 Bng 3.8 Nng hp ph ca cỏc mu kho sỏt 68 Bng 3.9 Cỏc thụng s ng nhit hp ph Langmuir v Freundlich ca Graphen oxit v Graphen ca As(V) 69 Bng 3.10 Phõn loi s phự hp ca mụ hỡnh ng nhit bng tham s RL 70 Bng 3.11 Giỏ tr tham s cõn bng RL ca quỏ trỡnh hp ph bng graphen oxit v graphen 71 Bng 3.12 S ph thuc lnqe vo lnCe i vi mụ hỡnh Freundlich 72 Ngụ Quang Binh iv Lun thc s DANH MC CC HèNH V Hỡnh 1.1 Cu trỳc tinh th kim cng Hỡnh 1.2 Cu trỳc tinh th graphit (Than chỡ) Hỡnh 1.3 Mụ hỡnh Fulleren Hỡnh 1.4 Mụ hỡnh ng nano cacbon Hỡnh 1.5 Cu trỳc ca ng nanocacbon n vỏch (a) v a vỏch (b) Hỡnh 1.6 Graphen - vt liu cú cu trỳc c bn (2D) cho cỏc vt liu cacbon khỏc (0D, 1D, v 3D) Hỡnh 1.7 Cu trỳc lp ca tinh th graphen Hỡnh 1.8 Graphen n lp 10 Hỡnh 1.9 Graphen a lp 10 Hỡnh 1.10 Phng phỏp tỏch lp graphit bng bng dớnh 13 Hỡnh 1.11 C ch to mng graphen bng phng phỏp nung nhit SiC 15 Hỡnh 1.12 K thut ch to graphen t CVD 17 Hỡnh 1.13 a- quỏ trỡnh oxi húa t graphit thnh graphen oxit 17 b-quỏ trỡnh kh graphen oxit bng hydrazin c sut 17 Hỡnh 1.14 nh minh qui trỡnh tỏch lp graphit dung dch, khụng oxi húa 19 Hỡnh 1.15 Hỡnh nh minh mng graphen oxit 22 Hỡnh 1.16 Cu trỳc ca graphen oxit (GO) theo mụ hỡnh ca Lerf Klinowski 23 Hỡnh 1.17: Liờn kt hydro gia cỏc lp graphit oxit 24 Hỡnh 1.18 nh hng ca nhit lờn hp ph v hp ph hot ng 32 Hỡnh 2.1 Tỏch lp siờu õm c hc 38 Hỡnh 2.2 Graphit oxit trc (A) v sau (B) vi súng 38 Hỡnh 2.3 S kh nhit GO 39 Hỡnh 2.4 Tng hp nano composit Fe3O4-GO bng phng phỏp ng kt ta 40 Hỡnh 2.5 ng i ca tia Rnghen 41 Hỡnh 2.6 S nguyờn lý s to nh phõn gii cao TEM 45 Ngụ Quang Binh v Lun thc s Hỡnh 2.7 Cỏc dng ng ng nhit hp ph-kh hp ph theo phõn loi ca IUPAC 46 Hỡnh 2.8 th biu din s bin thiờn ca P/[V(Po - P)] theo P/Po 47 Hỡnh 3.1 Ph XRD ca nguyờn liu u v sau oxi húa 50 Hỡnh 3.2 Ph XRD ca GO sau c oxi húa cỏc t l Graphit/ KMnO4 cỏc t l 51 Hỡnh 3.3 Ph XRD ca GO vi cỏc iu kin nhit ca quỏ trỡnh tng hp khỏc 52 Hỡnh 3.4 Thit b tng hp GO bng k thut vi súng 53 Hỡnh 3.5 Ph XRD v FT-IR ca graphen cỏc iu kin nhit nung khỏc 56 Hỡnh 3.6 Ph XRD ca graphen oxit v graphen sau tng hp 57 Hỡnh 3.7 Ph FT-IR ca graphen oxit v graphen sau tng hp 58 Hỡnh 3.8 nh HR-TEM ca graphen oxit siờu õm (a), Graphen oxit vi súng (b) v graphen (c) 60 Hỡnh 3.9 ng ng nhit hp ph - kh hp ph N2 77K (a, c) v ng phõn b kớch thc mao qun (b, d) ca graphen oxit v graphen 61 Hỡnh 3.10 Ph XPS ca graphen oxit siờu õm v graphen 63 Hỡnh 3.11 C ch ngh cho quỏ trỡnh kh nhit t graphen oxit v graphen 65 Hỡnh 3.12 nh hng pH n quỏ trỡnh loi b As (V) trờn vt liu GO v Fe3O4/GO, (nng As 7ppm, m/V= 0,4g/L, T=30oC) 66 Hỡnh 3.13 ng hp ph ng nhit Langmuir ca As(V) trờn graphen oxit v graphen 68 Hỡnh 3.14 Giỏ tr RL ph thuc vo nng As(V) ban u 71 Hỡnh 3.15 ng hp ph ng nhit Freundlich ca As(V) trờn graphen oxit v graphen 72 Hỡnh 3.16 ngh c ch hp ph As(V) lờn trờn vt liu hp ph GO 74 Hỡnh 3.17 Dựng nam chõm thu hi vt liu Fe3O4/GO 74 Ngụ Quang Binh vi Lun thc s TI LIU THAM KHO Ti liu tham kho ting Vit V ỡnh C, T Hc NXB khoa hc k thut Hunh Th M Hoa (2010), Ch to v kho sỏt tớnh cht c trng ca graphene, lun thc s, thnh ph H Chớ Minh Nguyn Hu Phỳ (1998), Giỏo trỡnh hp ph v xỳc tỏc trờn b mt vt liu v vụ c mao qun, Nh xut bn khoa hc v k thut, H Ni Phm Th Thm 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