Cc phng php ch to mng bn dn Trong chng ny, chng ti gii thiu phng php nghin cu thc nghim s dng

trong qu trnh nghin cu kho lun. l phng php ch to mng mng da trn nguyn tc phn x catt. 2.1- Phng php phn x catt (Cathode sputtering method). Phn x catt l mt trong nhng phng php c dng ph bin nht hin nay trong cc phng th nghim ch to vt liu di dng mng mmg. Phng php ny to c mng mng tng i hin a v i hi nhiu k thut do c thc hin trong bung chn khng cao (p sut phi thp hn 106

Torr). Mng mng to bi phng php ny c cht lng rt tt nh

sch, ng nht cao, nh hng tt, dy ln v iu khin c. 2.1.1 - Cu to. Thit b gm ba phn c bn: H bm chn khng, ngun pht cao tn v bung mu

Hnh 2.1:My to mng bng phng php phn x 2.1.2- Hot ng.

C s ca phng php phn x catt c thc hin da trn hin tng bn ph ca cc ht c nng lng cao vi cc nguyn t ca cht rn lm bia (c gn vi catt),lm bt cc nguyn t ca bia ra hng ti (c gn vi ant) ri lng ng thnh mng. Cc nguyn t dng bn ph thng l kh tr Argon hoc hn hp kh Argon vi kh kch hot (reactive gas)l oxi hay nit. Phn x c th thc hin theo ch phn cc DC hoc ch cao tn rf (magnhetron hoc khng magnhetron). Trong phng php ny mng mng ZnO a tinh th thng c to ch phn x r.f magnhetron trong mi trng kh Argon vi bia l gm c to ra t bt ZnO nung thiu kt. Ch to mng ny tit kim c nng lng,cc ht ti c nng lng cao do to ra mng cht lng tt, chc c v nh hng cao

Hnh 2.2: nh Plasma 2.1.3- Phng php sol-gel. + Phng php sol-gel do R. Roy xut nm 1956 cho php trn ln cc cht quy m nguyn t.Do sn phm thu c c ng nht v tinh khit rt cao, b mt ring ln, di ph phn b kch thc ht hp. Bn cht ca phng php sol-gel l da trn cc phn ng thu phn v ngng t tin cht (precusor) bng cch iu

chnh tc ca hai phn ng thu phn v ngng t chng ta s t c vt liu mong mun. T dung dch (sol) ban u bao gm cc cht a vo phn ng c ho tan vi nhau, phn ng thu phn ngng t ta thu c gel, sau sy c xerogel (sy siu ti hn hoc chng ct ng ph c aerogel), nung nhit thch hp c vt liu mong mun. Qu trnh sol-gel c th cho ta gel cha tan b cc cht tham gia phn ng v dung mi ban u, hoc kt ta gel tch khi dung mi v c khi l c cc cht sau phn ng. Vi a s cc phn ng th tc phn ng thu phn thng ln hn tc phn ng ngng t. V vy nghin cu v ng hc phn ng iu chnh cho tc ca hai phn ng xy ra thch hp vi cht sn phm cui. Hin nay, phng php sol-gel c pht trin theo hai hng chnh: - Phng php sol- gel theo con ng thu phn mui. - Phng php sol-gel theo con ng thu phn alkoxyde. - Phng php sol-gel theo con ng to phc. 2.1.4 - Phng php bc bay trong chn khng. Phng php ny da trn nguyn tc lm nng chy v bay hi (hoc thng hoa) trong bung chn khng cc nguyn t cht rn lng ng, cc nguyn t ho hi ln b mt rn. Tc nhn lm bc bay c th l do nhit lng Joule do t nng thuyn, chm in t nng lng cao hay chm laze lin tc (hoc laze xung). Vt liu bc bay c th l chnh dung dch rn hoc cc cht thnh phn ca vt liu mng. Hu ht cc cht bn dn A2B6 c th nhn c bng phng php ny vi sch cao, ng nht cao, kim sot c dy v tnh hp thc ca mng.

Mng ZnO c th c to bng cch bc bay nhit trc tip mui km acetate ZnO(CH3COO)2 hoc bc bay kim loi km nguyn cht sau oxy ho mng Zn trong mi trng oxy nhit cao. 2.1.5- Phng php lng ng ho hc t pha hi. Hi ca bn dn thnh phn c thi bng kh tr (N2 hoc Ar) t cc ng nng qua cc ng dn nng n bung phn ng oxy v hi nc cng c nn vo trong . Phng php ny d thc hin nhng c sch khng cao. 2.2- H o hunh quang. 2.2.1- Cu to. H FL3-22 l mt h o quang ph bao gm hai my n sc s dng cch t kp c phn gii 0.2 mm. + n sc 1 gi l n sc kch thch (Excitation Spectrometer ) dng thay i bc sng kch thch vo mu t 250 nm n 900 nm. + n sc 2 gi l n sc bc x (Excitation Spectrometer ) phn tch tn hiu pht ra t mu bn dn. Khong tn hiu n c th thu nhn phn tch l 350 nm n 850 nm. nh sng kch thch mu c ly t mt n Xenon qua n sc + n Xenon c cng sut ln (450 W ), nui bng ngun 25 (A), do n c t trong mt hp bo v v lm ngui bng qut. + B nhn quang in 1911 F c tc dng thu nhn tn hiu pht ra v khuych i tn hiu ln. + B tch sng tn hiu chun DM 320. + B x l SAC c tc dng phn tch tn hiu thu c v iu khin t ng h FL3 22.

Tn hiu c x l bng my tnh 2.2.2 - Hot ng. nh sng t n Xenon qua n sc 1 ti mu, tn hiu pht ra i qua n sc 2 v thu nhn bi b nhn quang in 1911 F. Tn hiu t b nhn quang in ny c a qua b tch sng tn hiu chun DM320. Sau a vo b x l SAC. Cui cng tn hiu c x l s a vo my tnh ghi nhn v lu li. 2.2.3 - Phng php o hunh quang. +o hunh quang pht x: ta c nh bc sng kch vo mu (cm) ly t n sc mt, qut bc sng ca n sc 2. Ph hunh quang thu c cho ta s ph thuc ca tn hiu pht ra t mu vo bc sng. +o hunh quang ph kch thch: ta chn v c nh bc sng ca n sc 2, qut cc bc sng kch thch. Do v tr cc i ca ph hunh quang kch thch cho ta bit ti v tr bc sng kch thch no th ph hunh quang mnh nht. iu ny c ngha nh ph kch thchex ng vi nh ph hp th 2.3- H o ph hp th phn t UV-VIS. 2.3.1- Cu to. o ph hp th phn t UV-VIS ta cn c 1 my ph UV-VIS. My quang ph hin i hay n gin n cng bao gm nhng b phn chnh sau: + Ngun cung cp chm sng (photon ) UV-VIS hay UV hoc VIS + Bung t cuvet v cuvet cha mu o.

+ B n sc ( h o quang hc ) thu ph, phn ly v chn tia sng o. + Detector v modun in t. + My hay trang b ghi nhn v ch th kt qu o ph.

Hnh 2.3 nh my o UV-VIS 3101 2.3.2- Hot ng. + Ngun sng:Trong cc my o ph UV-VIS (trc quang ) thng l n h quang hyro nng D2-Lamp, cho ph vng t ngoi (UV:190-360 nm), v n W-Halid cho ph vng kh kin (380-1000nm ) hoc n Xenon (260-600nm). Hin nay ph bin nht l 2 loi n D2 v W cho vng ph UV-VIS. Cc loi n ny l cc ngun sng im. N l ngun nng lng kch thch cc cht sinh ra ph hp th UV-VIS. + B phn detector: L b phn nhn v pht hin chm sng.Trong cc my n gin ngi ta dng t bo quang in. Trong cc my i c nhy cao thng dng cc nhn quang in kiu ng c nhy cao,v hin nay mt s my dng Detector Diod array. 2.3.3- Nguyn tc ca php o ph UV-VIS. +Nu cht phn tch l c ph ht th UV-VIS, th ta ho tan n vo trong mt dung mi ph hp, nh mt s cht hu c:

phenon naphathalen, anthracene. Cc cht v c I2, cc mui K2CrO4,K2CrO7. Nu mu phn tch l cht kh, th phi cha mu vo trong mt ng cuvet ng kn t trong bung o ph. + Chiu vo cuvet c dung dch mu cha hp cht cn phn tch 1 chm tia sng c nng lng ph hp cho cht phn tch hay sn phm phc ca n hp th bc x , to ra ph ht th UV-VIS ca n. V th cht phn tch ( mu phn tch ) cn c ng vo ng o hay cuvet c b dy nht nh (L=0.5;1, hay 2cm). Hay qut ph hp th. + Thu chm sng i qua cuvet, phn ly ph v chn mt hay hai sng hp th cc i ca cht phn tch v o cng hp th quang A ca cht trong cc iu kin chn. + Ghi gi tr hp th quang A.. Vic ny c th c thc hin bng nhiu cng c khc nhau, nh ng h o nng lng, my t ghi, ghi hp th A di dng cc pc hp, hay hin kt qu o A bng my hin s ( digital ). chnh l nguyn tc ca php o ph hp th phn t UV-VIS.