I HC QUC GIA H NI TRNG I HC KHOA HC T NHIấN - - Trnh Xuõn S CH TO MNG NANO KIM LOI QUí V TèM HIU KH NNG NG DNG LUN VN THC S KHOA HC H Ni, Nm 2014 I HC QUC GIA H NI TRNG I HC KHOA HC T NHIấN - - Trnh Xuõn S CH TO MNG NANO KIM LOI QUí V TèM HIU KH NNG NG DNG Chuyờn ngnh: Vt lý cht rn Mó s: 60440104 LUN VN THC S KHOA HC NGI HNG DN KHOA HC: PGS.TS Nguyn Hong Hi H Ni, Nm 2014 LI CM N Li u tiờn, em xin gi li cm n chõn thnh v sõu sc nht PGS.TS Nguyn Hong Hi, ngi ó ó tn tỡnh hng dn v to iu kin giỳp em hon thnh lun ny Xin by t lũng cm n sõu sc n anh Lu Mnh Qunh ó úng gúp nhng ý kin quý bỏu sut quỏ trỡnh thớ nghim v hon thin lun Em cng gi li cm n chõn thnh ti cỏc Thy, Cụ, cỏc anh ch v cỏc bn hc viờn thuc B mụn Vt lý Cht rn, Trung tõm Khoa hc Vt liu, khoa Vt lý ca Trng i hc Khoa hc T nhiờn i hc Quc Gia H Ni ó h tr, to iu kin v úng gúp ý kin quý bỏu v kt qu ca lun Cui cựng, em xin gi li cm n chõn thnh ti bn bố v nhng ngi thõn gia ỡnh ó luụn ng viờn, giỳp em sut quỏ trỡnh hc cng nh hon thnh lun H Ni, thỏng 12 nm 2014 Hc viờn Trnh Xuõn S MC LC M U 11 Chng 1: TNG QUAN Error! Bookmark not defined 1.1 Gii thiu v Platin Error! Bookmark not defined 1.1.1 Tớnh cht vt lý Error! Bookmark not defined 1.1.2 Tớnh cht húa hc Error! Bookmark not defined 1.1.3 Mt s hp cht Platin Error! Bookmark not defined 1.1.4 Cỏc ht nano Pt Error! Bookmark not defined 1.2 Cỏc phng phỏp ch to mng Pt Error! Bookmark not defined 1.2.1 Phng phỏp bc bay nhit Error! Bookmark not defined 1.2.2 Phng phỏp bc bay chựm in tError! Bookmark not defined 1.2.3 Phng phỏp phỳn x catot Error! Bookmark not defined 1.2.4 Phng phỏp lng ng pha hi húa hc (CVD) Error! Bookmark not defined 1.2.5 Phng phỏp m in húa Error! Bookmark not defined 1.2.6 Phng phỏp m húa hc Error! Bookmark not defined 1.2.7 Phng phỏp polyol Error! Bookmark not defined 1.3 Cm bin sinh hc Error! Bookmark not defined 1.3.1 Gii thiu v cm bin sinh hc Error! Bookmark not defined 1.3.2 Cm bin sinh hc in húa Error! Bookmark not defined 1.3.3 ng dng mng Platin cm bin sinh hc Error! Bookmark not defined 1.4 Phng phỏp v nh hng nghiờn cuError! defined Bookmark not Chng 2: THC NGHIM Error! Bookmark not defined 2.1 Ch to mng Pt Error! Bookmark not defined 2.1.1 Cỏc húa cht v thit b s dng Error! Bookmark not defined 2.1.2 Quy trỡnh ch to Error! Bookmark not defined 2.2 Chc nng húa b mt mng Pt v gn kt vi cỏc phõn t sinh hc Error! Bookmark not defined 2.2.1 Húa cht Error! Bookmark not defined 2.2.2 Chc nng húa b mt mng Pt Error! Bookmark not defined 2.2.3 Gn kt enzyme v axit citric Error! Bookmark not defined 2.3 Cỏc phng phỏp phõn tớch v kho sỏtError! Bookmark not defined 2.3.1 Phng phỏp nhiu x tia X Error! Bookmark not defined 3.3.2 Kớnh hin vi in t quột (SEM) Error! Bookmark not defined 2.3.3 Ph tỏn sc nng lng tia X (EDX)Error! Bookmark not defined 2.3.4 Kớnh hin vi lc nguyờn t (AFM)Error! Bookmark not defined 2.3.5 Phng phỏp o biờn dng bng u dũ hỡnh kim Error! Bookmark not defined 2.3.5 Phng phỏp phõn tớch ph hng ngoi (IR)Error! Bookmark not defined 2.3.6 Phng phỏp tỏn x Raman Error! Bookmark not defined Chng 3: KT QU V THO LUN Error! Bookmark not defined 3.1 Kt qu ch to mng Pt Error! Bookmark not defined 3.1.1 Phõn tớch cu trỳc Error! Bookmark not defined 3.1.2 Phõn tớch thnh phn Error! Bookmark not defined 3.1.3 Hỡnh thỏi v kớch thc Error! Bookmark not defined 3.1 Mt s tớnh cht khỏc Error! Bookmark not defined 3.2 Kt qu chc nng húa mng Pt Error! Bookmark not defined 3.2.1 Kt qu FTIR Error! Bookmark not defined 3.2.2 Ph Raman Error! Bookmark not defined 3.3 Gn kt cỏc phõn t sinh hc Error! Bookmark not defined 3.3.1 Gn kt enzyme Error! Bookmark not defined 3.3.2 Gn kt vi axit citric Error! Bookmark not defined KT LUN Error! Bookmark not defined TI LIU THAM KHO 13 DANH MC Kí HIU V CC CH VIT TT CVD (chemical vapor deposition) Lng ng pha hi húa hc XRD (X-Ray Diffraction ) Nhiu x tia X SEM (Scanning Electron Microscope) EDX hoc EDS (Energy-dispersive X-ray spectroscopy) Kớnh hin vi in t quột Ph tỏn sc nng lng tia X AFM (Atomic force microscopy) Kớnh hin vi lc nguyờn t FTIR (Fourier transform infrared Quang ph hng ngoi chuyn i spectroscopy) Fourier SAM (self-assembled monolayer) n lp t sp xp 4-ATP 4-Aminothiophenol EDC 1-Ethyl-3-(3-dimethylaminopropyl) ethylcarbodiimide PBS Phosphate-buffered saline EG Ethylene glycol GA Glycolaldehyde DANH MC HèNH V Tờn hỡnh v Trang Hỡnh 1.1 Mt s phng phỏp ch to mng mng Hỡnh 1.2 S h bc bay nhit Hỡnh 1.3 S h bc bay chựm in t 10 Hỡnh 1.4 S h phỳn x 11 Hỡnh 1.5 S phng phỏp CVD 13 Hỡnh 1.6 S phng phỏp m in 14 Hỡnh 1.7 Cỏc b phn chớnh ca mt cm bin sinh hc 20 Hỡnh 1.8 Mụ hỡnh mng sau c chc nng húa 24 Hỡnh 2.1 S ch to mng Pt bng phng phỏp kh polyol 29 Hỡnh 2.2 Nhiu x tia X 31 Hỡnh 2.3 Thit b kớnh hin vi in t quột Jeol 5410 LV ti Trung tõm Khoa hc Vt liu 33 Hỡnh 2.4 Mụ hỡnh o kớnh hin vi lc nguyờn t 35 Hỡnh 2.5 S h o biờn dng u dũ hỡnh kim 36 Hỡnh 3.1 Gin nhiu x mng Pt trc nhit 40 Hỡnh 3.2 Gin nhit x ca mng Pt nung cỏc nhit khỏc 41 Hỡnh 3.3 Ph EDX ca mu trc nung 43 Hỡnh 3.4 Ph EDX ca mu nung 450C 43 Tờn hỡnh v Hỡnh 3.5 nh SEM mng Pt ch to 140C trc nung Hỡnh 3.6 nh SEM mng Pt ch to 140C sau nung 450C (a) cu trỳc mng, (b) cỏc ỏm ht Trang 44 44 Hỡnh 3.7 nh SEM mu ch to 160C 46 Hỡnh 3.8 nh AFM ca mu ch to 140C sau nung 46 Hỡnh 3.9 Kt qu o dy mng bng Alpha-Step 47 Hỡnh 3.10 Ph FTIR (a) 4-ATP trờn Silic (b) mng Pt sau c chc nng húa bng 4-ATP Hỡnh 3.11 Hỡnh nh mụ t mng Pt sau c chc nng húa Hỡnh 3.12 Ph Raman ca mng Pt v mng Pt sau chc nng húa bng 4-ATP Hỡnh 3.13 Ph FTIR ca mng Pt gn kt enzyme Hỡnh 3.14 Ph FTIR ca mng Pt gn axit citric thang o (a) 500 4000 cm-1 (b) 1200 2200 cm-1 49 50 51 53 55 DANH MC BNG BIU Tờn Bng Trang Bng 2.1 Danh sỏch cỏc húa cht s dng 29 Bng 3.1 Cỏc kt qu tớnh kớch thc ht theo cỏc nh nhiu x 40 Bng 3.2 Kt qu cỏc kớch thc ca ht nhit 300C 41 Bng 3.3 Kt qu cỏc kớch thc ca ht nhit 450C 42 Bng 3.4 V trớ cỏc mode dao ng ca 4-ATP nguyờn cht v mng Pt ó c chc nng húa Bng 3.5 V trớ nh Raman ca 4-ATP nguyờn cht v mng Pt sau c chc nng húa bng 4-ATP 50 52 M U Hin nay, lng ng mng kim loi ang l mt ch quan trng, thu hỳt c nhiu s quan tõm t c v ngoi nc Bờn cnh cỏc k thut lng ng thụng thng, cỏc phng phỏp tip cn mi liờn tc c tỡm hiu v nghiờn cu, ó khụng nhng gii quyt c nhiu khú khn trc õy m cũn tỏc ng mnh lờn kh nng ng dng ca mng kim loi thc tin Mt s nhng phng phỏp mi gõy c s chỳ ý gn õy l phng phỏp lng ng mng kim loi s dng phn ng kh mui Chỳng ta bit rng cỏc phn ng húa hc kh mui cú th to kim loi nguyờn cht nhit thp Vỡ vy chỳng ó c ng dng rng rói ch to cỏc ht nano kim loi [26, 40, 47] nhng li rt him c s dng vic lng ng mng hin tng cỏc mm kim loi thng hỡnh thnh v ln lờn lũng cht lng v to thnh ht kim loi thay vỡ thnh mng Tuy nhiờn nu kim soỏt cho mm kim loi hỡnh thnh v phỏt trin trờn b mt cht nn thỡ cú th thu c mng kim loi vi cht lng tt nhit thp Platin l mt kim loi quý, cú nhiu ng dng quan trng cỏc lnh vc khỏc Pt cú tớnh tr, rt ớt b n mũn, dn in tt v kh nng xỳc tỏc hiu qu nhiu phn ng húa hc, nờn thng c s dng cỏc h thng chuyn i nng lng nh pin nng lng mt tri [41, 50, 56, 59, 65], t bo nhiờn liu (fuel cells) [3, 7, 19, 53, 57] v c cm bin sinh hc [3, 35, 38] Trong nhiu ng dng, Pt thng dựng di dng mng Mng Pt cú th c lng ng bng nhiu phng phỏp húa lý khỏc Nú cú th c ch to t kim loi Pt nguyờn cht s dng phng phỏp phỳn x magnetron [39, 57], lng ng pha hi húa hc [32, 49, 56] bc bay chựm in t hay bc bay nhit Nú cng cú th ch to t dung dch mui Pt hay axit chloroplatinic s dng phng phỏp lng ng in húa [12, 61] hoc m húa hc [14, 15, 31, 72] Mi phng phỏp ny u cú nhng gii hn v nhc im riờng Chng hn, phỳn x magnetron v bc bay chựm in t yờu cu chõn khụng v nng lng cao, lm tng ỏng k chi phớ ch to Lng ng in húa thỡ cn cú dn tt v n nh cao dung dch in gii, ú lng m húa hc li cn mt lp kim loi hot ng trờn b mt ca cht nn Trong thi gian gn õy, phng phỏp kh polyol mui Pt bt u c s dng rng rói lng ng mng Pt õy l phng phỏp n gin ch s dng cỏc phn ng húa hc thun tỳy nờn chi phớ r, khụng yờu cu cỏc thit b phc hay mụi trng ch to c bit, m thu c mng kim loi cú cht lng tt, thớch hp cho nhiu ng dng khỏc Trc ú, phng phỏp polyol ch yu dựng ch to cỏc ht nano kim loi [10, 60, 63], rt ớt nghiờn cu vic ch to mng Kurihara v cỏc ng s ó cú mt bỏo cỏo ngn gn v lng ng mng kim loi bao gm Co, Ni, Rh, Re,W, Pt, v Au trờn nn cỏc khụng dn khỏc nh pyrex, kapton, teflon, si graphit, si cacbon, bng cỏch nhỳng cỏc ny vo hn hp dung dch phn ng ca mui kim loi [44] Mng sau ch to cú cu trỳc nano vi kớch thc tinh th trung bỡnh khong 10 nm Hin nay, ó cú nhiu cụng trỡnh trỡnh s dng phng phỏp kh polyol lng ng mng Pt nh mt phng phỏp n gin v tit kim [41, 65, 66] Tuy nhiờn a s cỏc nghiờn cu ny u ch trung ng dng vo pin mt tri, gn nh cha cú mt bỏo cỏo no th nghim ng dng nhng lnh vc khỏc, c bit l lnh vc sinh hc Vỡ vy nhm mc ớch tỡm hiu, chỳng tụi tin hnh nghiờn cu cỏc tớnh cht ca mng Pt c ch to bng phng phỏp polyol trờn silic ng thi th nghim ng dng ch to cm bin sinh hc vi tờn ti ca lun l: Ch to mng nano kim loi quý v tỡm hiu kh nng ng dng Trong lun vn, chỳng tụi s dng polyol l ethylene glycol kh mui H2PtCl6 to mng Pt trờn silic Mng sau to thnh c x lý nhit phõn hy ht cỏc thnh phn hu c cũn sút li ng thi tng cng bỏm dớnh lờn Cỏc c tớnh cu trỳc, hỡnh thỏi v tớnh cht c nghiờn cu mt cỏch c th v chi tit Cui cựng mng c th nghim ch to cm bin sinh hc thụng qua nghiờn cu kh nng chc nng húa b mt v kh nng ớnh kt vi mt s phõn t sinh hc Nh vy mc tiờu chớnh ca lun c t ra: - Ch to mng nano Pt bng phng phỏp kh polyol - Nghiờn cu cu trỳc, hỡnh thỏi b mt v tớnh cht ca mng c to thnh - Th nghim kh nng ng dng ch to cm bin sinh hc Lun c chia lm cỏc phn: Chng I: Tng quan cỏc phng phỏp ch to mng Pt, tớnh cht ca Pt v gii thiu v cm bin sinh hc Chng II: Thc nghim Quy trỡnh ch to mng Pt, chc nng húa 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