Formation of ZnO in or on glasses by using the Sol-Gel and Chemical Bath Deposition Techniques

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1 Formaton of ZnO n or on glasses by usng the Sol-Gel and Chemcal Bath Deposton Technques S. J. CASTILLO 1, M. C. ACOSTA-ENRÍQUEZ 1, MA. E. ZAYAS 1, H. ARIZPE 1, T. MENDÍVIL- REYNOSO 1, A. GARCIA-JUÁREZ 1, M. E. ALVAREZ-RAMOS AND E. LARIOS- RODRÍGUEZ 3,4 1 Departamento de Investgacón en Físca, Unversdad de Sonora, Apdo. Postal 5-88, CP. 83, Hermosllo, Sonora, Méxco. Departamento de Físca, Unversdad de Sonora, Apdo. Postal 166, CP. 83, Hermosllo, Sonora, Méxco. 3 Departamento de Investgacón en Polímeros y Materales, Unversdad de Sonora, CP. 83, Hermosllo, Sonora, Méxco. 4 Departamento de Ingenería Químca de la Unversdad de Sonora, CP. 83, Hermosllo, Sonora, Méxco. semconductores@dfus.uson.mx Abstract: - In the frst part of ths work was produced Znc Oxde (ZnO) nto a glass matrx by usng the Sol- Gel Technque at room temperature, these materals were prepared usng tetraethyl orthoslcate (TEOS) as precursor, the Zn ons were added before the jellfcaton step trough an aqueous soluton of znc acetate. These glasses were characterzed by X-ray dffracton, optc absorpton, FT-IR and Raman spectroscopy. The X-ray patterns showed amorphousness. The optcal absorpton shows a shoulder n the UV range correspondng wht ZnO confned to the vtreous matrx. The spectra by FT-IR show characterstc vbratons of S-O-S wth nteracton Zn +. Raman scatterng let us to dentfy and precse the formaton of the ZnO. In the second part of ths work was mmersed glass substrates nto an aqueous chemcal bath wth external controlled temperature, the chemcal solutons contaned n the bath were a Zn Ions source (ZnSO 4 ).1 M, a ph 1 Buffer soluton (NH 4 Cl/NH 4 OH), Ethanolamne to complex the Zn ons, and pure water, resultng ZnO flms hexagonally structured wth energy band gap of 3.3 ev, growng 1 nm durng 5 mnutes followed of 6 mnutes to 75 C and 85 C n the same chemcal reacton. Key-words: Glasses, Zn Ions, Znc Oxde, Sol-Gel Process, Thn Flms, Chemcal Bath Deposton and semconductors 1 Introducton Znc oxde has attracted a sgnfcant attenton n the last decades because ts wde band gap behavor whch confers a host of potental applcatons n gas sensors [1], solar cells [, 3], Catalyss [4], Organc lght emttng dodes (OLEDs) [5], mcroelectronc devces how transstors [5-9], partcularly a very nterestng use of the ZnO s lke electronc devces wth hghly nonlnear current-voltage relatonshps called Varstors [1-14]. At small appled electrc felds, varstors are nsulatng; but at a farly welldefned hgher feld, those swtch to conductng and mantan a nearly constant feld over many decades or magntude orders of current. Most commercal, and mltary applcaton varstors are based on polycrystallne, semconductng ZnO wth a varety of other oxde addtves typcally n the molar range of 1 parts per mllon to several percent. Ther man applcaton s n electrcal crcuts to lmt or regulate the voltage that can be appled to other devces or components. Whle t s common for varstors to operate wth current denstes of 1-3 to 1 A/cm, some others applcatons also requre unusually hgh electrc felds near 4kV/cm. Wth these hgh power condtons, t s perhaps not surprsng those small flaws n the varstor result n breakdown, or a large rreversble change n ther electrcal and sometmes structural propertes. The functonal dependence of current on voltage n these devces s symmetrcally bpolar that s due to an nherent property of the semconductor from whch t s made. Several process usng both chemcal and physcal methods have been reported for the producton of these materals (ZnO and ZnO-compostes) lke tape castng[14], sol-gel[15-16], vapor-phase transport ISSN: Issue 3, Volume 9, March 1

2 method[17], chemcal vapour transport (CVT) process, spray pyrolyss (SP)[18], sputterng, etc., ether to produce powders, thn flms, nanopartcles, nanorods, compostes, etc. Partcularly ZnOcompostes ether usng a matrx of glass, ceramc or polymerc, are very attractve snce these compostes offer many possbltes for creatng new materals, especally for mcroelectroncs and nanoelectroncs ndustry, because through approprate technques can be homogeneously dsperse the partcles of the semconductor (ZnO) n the matrx chosen. Furthermore, ZnO thn-flm transstors (TFT) have recently receved much attenton due to ther potentals toward a new drvng component for lqud crystal dsplay and other applcatons lke solar cells, etc. The purpose of ths work s to study two alternatve ways to prepare compostes contanng SO glasses and Zn ons or ZnO molecules. The frst one, by usng the sol-gel technque, s a way to prepare ths knd of the requred compostes startng from TEOS as precursor, then the Zn ons are added trough an aqueous soluton of Zn(CH 3 COO) H O n the process, before the gel formaton. The process s carry on at room temperature and the complete process s as smple as the sol-gel technque. The second one, by Chemcal Bath Deposton (CBD) technque usng two reacton temperatures T 1 =75 C and T = 85 C, durng respectve tmes of 5 mnutes and 1 hour, n the same reacton. Materals and Methods The used chemcals compounds were reagent grade, but wth purtes between 98 to 99%. For the frst compostes were used Deonzed Water, Absolute Ethanol, Tetraethyl Orthoslcate, Chlorhydrc Acd and Znc Acetate. For the second compostes knd were used Deonzed Water, Znc Sulfate, Buffer Soluton ph 1 (NH 4 OH/NH 4 Cl), Ethanolamne and Cornng brand mcroscope sldes as substrates..1 Expermental Method to produce ZnO nto a glass matrx by usng the Sol-Gel Technque Ten samples wth dfferent proportons of znc ons were prepared, where the ZnO sngle molecules or nanopartcles were formed beng embedded nto the SO phase. The startng solutons were prepared by mxng TEOS, water and ethanol. Ths set of samples was prepared usng a constant ethanol:teos volume rato of 1:1 and a volume rato of water : TEOS, 1:1. The soluton was catalyzed wth 5 drops of concentred HCl (or some dluton), n order to homogenze ts phases, Sol formaton. It s necessary to wat several days (7-15) to dry the monolths. After jellfcaton all samples were dred and/or ground to obtan a fne powder at room temperature. The znc was ncorporated nto the samples, dssolvng Zn (CH 3 -COO) nto water and added to the startng soluton. The amount of the znc acetate vared from.1 M to 1. M, see Table 1. Sample TEOS PureEthanol ZnAc Dhydrated 1 1 ml 1 ml 1 ml,.1 M 1 ml 1 ml 1 ml,. M 3 1 ml 1 ml 1 ml,.3 M 4 1 ml 1 ml 1 ml,.4 M 5 1 ml 1 ml 1 ml,.5 M 6 1 ml 1 ml 1 ml,.6 M 7 1 ml 1 ml 1 ml,.7 M 8 1 ml 1 ml 1 ml,.8 M 9 1 ml 1 ml 1 ml,.9 M 1 1 ml 1 ml 1 ml, 1. M Table 1. Formulaton and proportons of the Samples. The label each sample means the tenths of molar concentraton n the sample. A D8 Brucker Advanced equpment dd the X-ray dfracton characterzaton, wth a Cu source of 1.54 Å. The optcal absorpton was done n an S- UV-VIS Ocean Optcs, Inc., and for the Raman spectroscopy was used a Raman Systems R-.. Expermental Method to produce ZnO on a glass substrate by usng the Chemcal Bath Deposton Technque The samples were prepared by deposton of znc oxde on glass substrate; we sent to analyze quanttatvely the chemcal composton of the substrates to a professonal lab n Tucson, Arzona USA, Desert Analytcs. In Table s the nformaton of that chemcal composton of the substrates, Cornng brand mcroscope sldes. ISSN: Issue 3, Volume 9, March 1

3 Element Concentraton Compound Concentraton Al.7 Al O S SO 7.8 Na 8.57 Na O Mg.478 MgO 4.18 S.17 SO.14 P P O 5 K.696 K O.839 Ca 4.7 CaO Fe FeO Mn MnO T.3 TO.5 O Stochometry - Total total Table. Quanttatve analyss and chemcal composton of the Substrates sent to analyze to a professonal lab n Tucson, Arzona USA, Desert Analytcs. Whereas, n Table 3 we tabulate the techncal nformaton of the provder of substrates. For oxdes, water normally provdes the oxygen. The processes that occur n the CBD soluton consst n general of the followng fve steps: (1) Tme zero to equlbrum between the complexng agent and water; () Hydrolyss of the chalcogende source (f the flm s not an oxde); (3) Formaton and/or dssocaton of onc metal lgand complexes [M(L) ] n-k, where L k- denotes one of more lgands, and (4), (5) Formaton of the solds. Step (4) conssts of the oxdaton of a metal hydroxde from the water release. Step (5) the controlled reacton of metallc catons ether wth onc oxygen or chalcogendes ons by mean of release complexng agents. Now schematcally, CBD for oxde or sulfde flms from a metal caton M n+ complexed by lgands L k-, can be depcted as follows (fve steps): 1) Dssocaton of water and Complexant-water equlbrum: nh O nh ( L) + + noh k k+ 1 + H O ( L) H OH + Composton Percent approx. SO 73% Na O 14% CaO 7% MgO 4% Al O 3 % Table 3 Techncal nformaton publshed for the provder of substrates. The chemcal bath deposton (CBD) s used for deposton technques that produce a sold flm n a sngle mmerson through control of the knetcs of formaton of the sold. Flm thckness and composton can be easly controlled by changng smple reacton parameters such as reactant concentraton, reacton temperature and deposton tme. The deposton medum for CBD conssts of one or more salts of metal M n+, a source for a chalcogende (f the flm to be deposted contans S, Se, etc), a source of oxygen for oxde flms and a complexng agent (e.g. ammona, NH 3, EDTA, sodum ctrate, etc.) all mxed n aqueous soluton. ) Thourea hydrolyzes to form sulfdes nsc( NH ) + noh ns + nch 3) Dsplacement of lgands: N + nh O ( n k ) + k noh + M ( L) M ( OH) n ( s) + ( L) 4) Deprotonaton to form oxdes n M ( OH) ( s) MOn ( s) + H n 5) Total Reactons: n ( n k ) + + k M ( L) + H O MOn ( s) + nh + ( L) ( n k) + k M ( L) + ns MSn ( s) + ( L) O ISSN: Issue 3, Volume 9, March 1

4 The complexant s optonal and s usually chosen based on the affnty of ts lgands toward the metal. Ths makes step 3 the rate-determnng step, addng a degree of control for thn flm thckness. The hydrolytc process of reactons 4 and 5 can be accelerated by heatng the soluton, whch nduces deprotonaton of the hydrated metal speces (reacton (4)). Ths elmnates the need to use a base n reactons 4 and 5. For the oxde systems to be formed n ths research work, hydrolyss can occur even n acdc solutons when the metal caton s easly hydrolysable, as n the case of some of the metals to be evaluated here (Al 3+, Zn +, In 3+ ). In contrast, CBD of non-oxdes requres the addton of basc solutons. In all CBD processes, whether oxde or non-oxde, a solvated metal complex reacts wth a chalcogende source to form a desred sold product. The man dfference s that for oxdes, the chalcogende source s water, so that tghter control must be exerted over just two parameters (ph, T) to acheve a smlar degree of control over the rate of hydrolyss and, therefore, control over the flm s mcrostructure and propertes. For non-oxde flms, the supply of chalcogende anons can be controlled, n addton to ph and temperature, wth the concentraton of the chalcogende source. The practcal procedure s too smple, conssts to mmerse the substrate nto the soluton (bath) contanng an aqueous soluton of complexed znc sulfate, untl the znc oxde thn flm s formed on the glass substrate. Reagents used to depost of ZnO thn flms n a two-stage temperatures process; 5 mnutes at 75 C and 1 hour at 85 C, n the same reacton bath: 36 ml of znc sulphate (ZnSO 4 ).1 M. Source metal. 1 ml of ph 1 controller buffer (NH 4 Cl/NH 4 OH). 18 ml of Dluted Ethanolamne n deonzed water, 5%:5%. Complexng agent. Complete to a volume of 1 ml wth deonzed water. Ths process has a sngular complcaton as reacton condton whch s: If we start to a ntal temperature lke the ambent, ~ 1 C, t s necessary to consder a frst reacton wth small temperature gradent, untl arrve to 75 C, 5 mnutes remanng n the latter, subsequently ncreasng the temperature to reach 85 C for 1 hour. Some equpment used to analyze ths second knd of composte were: X-ray dffracton was done n a Phlps X'Pert; studes of optcal absorpton UV -Vs was carred out usng a UV-Vs spectrophotometer brand Perkn Elmer, Model 33; the mage of the surface morphology, was performed wth a scannng electron mcroscope brand Topcon SM-51 (SEM); the Raman spectra were obtaned wth the equpment Mcro-Raman scatterng brand LABRAM-Dlor. The thckness was done drectly and enough accurate by usng a proflometer brand Dekatar. 3 Results Developed materals are of two types, so the presented results n ths secton wll try to mantan a systematc ndependence The monolths of slcon doxde wth embedded znc oxde partcles are amorphous, they scatter the lght and even some of them are opaque. The monolths ere characterzed by X-ray dffracton, UV-Vsble and Raman spectroscopes, whch below are explaned n some detal. Smlarly the growth Znc Oxde Thn flms on glass substrates led to a polycrystallne hexagonal structure, 1µm thckness and they were more completely characterzed by X-ray dffracton, vsble, Auger and Raman spectroscopes, and addtonally ts morphology was studed by scannng electron mcroscopy. 3.1 ZnO-Glass matrx compostes by Sol-Gel Technque (SO : ZnO) Let us to begn wth the commentary that the compostes obtaned had a dryng tme between 7 to 15 days. Also t s necessary to know that when added low proportons of znc acetate, the compostes were of a more translucent appearance, whereas that the obtaned compostes usng the hgher concentratons had opaque appearance. We could have to measured more features for ths materal, but t s necessary to break the research n order to report some partal results f not ths The XRD patterns obtaned showed that all the samples were amorphous compounds, as can be observed from Fg. 1. The behavor t s very smlar between each gel, bascally amorphous. However we can see that the wde band between θ = s better defned wth ncrease of content acetate of znc. A lttle peak appears at θ=34, samples correspondng to.8 and.9 M, whch can correspond to hexagonal ZnO structure. Here we can consder that the senstvty of the XRD ndcates the ZnO- Glass matrx compostes have ISSN: Issue 3, Volume 9, March 1

5 not crystallne partcles (SO : ZnO). Intensty (A.U.) 35 Glasses Contanng ZnAc1.M ZnO ZnAc.9M ZnAc.8M ZnAc.7M ZnAc.6M ZnAc.5M ZnAc.4M ZnAc.3M ZnAc.M ZnAc.1M O ptcal absor pton (A. U.) Wavel engh t (n m) 4 Glasses contanng ZnO Fg. Absorpton spectra of glasses wth znc ons (ZnO), n the 45-5 nm range. All the samples, except the number 7 show typcal ZnO behavor θ (Degrees) Fg1. XRD patterns of glasses wth znc ons (ZnO), showng essentally the amorphousness of the samples. In Fg. 3 are shown the absorpton spectra n the 45-64nm range, these spectra have a smlar behavor for almost all samples. In fact absorpton edges are weak n the zone of the 4-5 nm; from there the spectra behavor remans almost constant. The low ntenstes surely correspond wth the opaqueness and to the dspersve of most of the samples. Znc oxde has a wde drect band gap of slghtly bgger than 3 ev (~ 4 nm). It s a great UV absorber. The Fg. shows the absorpton spectra wth dfferent contents of acetate of znc. We can see an ncreasng of the optcal absorpton rsng from 3 nm toward UV regon n the graph. Ths plot also shows an absorpton edge located at about 4 nm, (the nflecton pont), whch means that ZnO s present n amorphous form n the samples. They showed opaqueness lead to a dffuse detecton of the ntensty by the UV-Vs spectroscopy technque, but any way the man behave follows the same features of the nvolved materal, we should not forget that ths ZnO formaton t s of very small and scattered partcles. Ths also corresponds wth the global amorphousness. Th e use d mo lar concentraton of O n th e sam ple t s correspondng to the label.15 Fg. 3 Absorpton spectra of glasses wth znc ons Op tcal absorpton (A. U.) W avelenght (nm ) Glas ses contanng ZnO (ZnO), n the nm range. Curously, the labeled samples 1 and begn an absorpton edge ISSN: Issue 3, Volume 9, March 1

6 around 5 nm. In the Fgure 4 s shown the IR spectrum of eght of the ten studed samples. In order to understand the orgn of the above glass structure n ths spectrum s observed an ntensve peak at 11 cm -1, whch can be attrbuted to characterstc vbraton of S-O-S brdges n the slca network [19-1]. The band seen at 965cm -1, can be related to the S-O-H stretchng vbraton [1-], ths peak ncreases as the concentraton of Zn decreases, whch s expected snce the sgnal of the slcon bonded to hydroxyl groups would be more ntense. The band at around 8 cm -1 observed for all the consdered concentratons, vary lkely due to nteracton between Zn + and the slca glass network whch can result between the two characterstc bands for slca at 8cm -1 and 47 cm Glasses Contanng ZnO ZnO Nano-Partcles (NPs) have dstnct physcal orgns to frst order so we can do such an analyss from the expermental Raman spectra of ZnO Bulkpowder (BP) and NPs, excted by 514.5nm laser lne, respectvely. The frst order Raman modes A1T, E1T, E (H), A1L and E1L are dentfed as the peaks at: 385, 46, 437, 57 and 584 c m 1 On other hand, Znc acetate n pure form shows a large peak n ts Raman Spectra, located at 96 cm -1, as t can be see Fg. 5. Ths peak s related wth CHout of plane molecular stretchng bond [4]. In our samples, ths peak could dsappear wth a thermal annealng, due to breakage of the organc bonds by heatng. Samples n pure powder at RT show two Raman small sgnals at 435 cm -1 and 556 cm -1 correspondng to reported n other works [3]. Both peaks have a small ntensty varyng for dfferent concentratons. The peaks at both postons are related wth oxygen vacances n ZnO []. ZnO can be derved n Sol-Gel procedures startng wth TEOS. In ths case, Raman spectra wll show a broad band rasng from 5 to 55 cm -1 correspondng to SO. Ths band can overlap the second mentoned Raman sgnal for ZnO. Intensty (A.U.) Decreasng Order Plots:. M.4 M.3 M.5 M.8 M.6 M.9 M.7 M Frecuency (cm -1 ) Fg. 4 Infrarred spectrum of our glasses wth znc ons (ZnO). From the Raman spectroscopy patterns can be dentfed a sgnal correspondng to ZnO, see Fgure 5, there are shown Raman spectra of as grown samples at room temperature; wth dfferent molar concentraton. Two broad bands are shown, correspondng to ZnO (435 cm -1 ) and SO, as we already apponted. As t can be seen, small molar concentratons result n larger peak ntenstes. The peak at 435 cm -1 s related wth E mode for ZnO. It s possble to use Raman Spectroscopy excted by laser lght of varous wavelengths to study LO and TO modes n polar and nonpolar semconductng materals, the frequency varatons of the LO and TO modes n polarzed semconductng materal lke Intensty (A. U.) Glasses Contanng ZnO Raman shft (cm -1 ) Fg. 5. Raman spectra of our glasses wth znc ons (ZnO). ISSN: Issue 3, Volume 9, March 1

7 3. ZnO Thn Flms on Glass substrate compostes by CBD technque (ZnO/Glass) Here we descrbe the specfc characterzaton developed to study our second materal, ths materal s norganc semconductor type metalchalcogende and t s obtaned n the form of thn flms by the method of chemcal bath deposton. Thanks to the versatlty of ths method or technque, t would be possble to vary a number of physcal and chemcal parameters that allow us to modfy the propertes of the obtaned semconductor. θ=47.53 o and 1.64Å to θ=56.6 o, whch correspond to the (1), (), (11), (1) and (11) planes of the hexagonal structure of znc oxde (JCPDS card ). Therefore, the materal syntheszed has the hexagonal phase of the Wurtzte structure (space group: p63 mc) of ZnO (calculated cell constants: a = 3.4 Å, c = 5. Å). The strong and sharp peaks ndcate that ths as syntheszed product s hghly crystallne and pure. Also, t can observe a wde band around θ=3 o, ths band corresponds to background of glass matrx (the substrate) (1) (11) Some Hexagonal ZnO peaks From a UV-Vs spectrometer we measure the absorbance, n Fg. 7. In ths case the flm s on the surface of the substrate, and then t can be measured or absorbance, or transmttance and also reflectance. We can to observe a fast ncreasng n the absorpton as we decrease the wavelength, n our study range, but an approprate data treatment and some theoretcal assumptons typcal, allows us to obtan the energy band gap. Intensty (A.U.) () (11). ZnO/Glass Sustrate 1 (1) θ (Degrees) Fg. 6. XRD pattern of our Znc Oxde Thn Flm on a glass substrate. Here can be observed the polycrystallne feature of the ZnO flm and the amorphous feature of the substrate, lke evolvng broad band. Optcal absorpton (A.U.) Wavelength (nm) The XRD pattern n Fgure 6 shows to us that the ZnO thn flm onto glass substrate was polycrystallne; the dffractogram dsplays several sharp peaks. These peaks are related to the lattce spacng s.814å to θ=31.77 o,.63å to θ=34.4 o,.475å to θ=36.5 o, 1.911Å to Fg. 7. Optcal Absorpton spectrum of our Znc Oxde Thn Flm on a glass substrate. Usng the fact that the ZnO s a drect bandgap semconductor, t s possble to calculate the Energy bandgap (Eg) by usng the optcal absorpton data. In ISSN: Issue 3, Volume 9, March 1

8 the Fg. 8 the absorpton data were treated and the Energy Band Gap was E g =3.3 ev Fg. 9. Detecton of some chemcal elements by Auger spectroscopy of our Znc Oxde Thn Flm on a glass substrate. [(Optcal Densty)(Energy)] (A.U.) Equaton y = a + b*x Adj. R-Square.994 Value Standard Error B Intercept B Slope From the Raman spectroscopy pattern seen n the Fg. 9, t s possble to observe a wde band between 54-6 cm -1, such has been reported as correspondng to the sgnal cm -1 of ZnO, wth hexagonal structure [5]. Ths broad band can be produced by the phonons A1 (LO) to 574 cm -1 and / or phonons E1 (LO) to 583 cm Energy (ev) Fg. 8. Plot for the energy band gap calculatons of our Znc Oxde Thn Flm on a glass substrate. E g =3.3 ev. Usng Auger spectroscopy we get the Fg. 9 where t s shown the presence of oxygen, znc and carbon. It s consdered that carbon s found as an envronmental contamnant snce CO t s absorbed by the flm. Ths confrms that DBQ s a very clean technque or selectve, snce t does not have other types of elements n the reagents. 6x1 6 5x1 6 4x1 6 ZnO 75 o C 85 o C Intensty (A.U.) Raman Shft (cm -1 ) Fg. 9. Raman shft of our ZnO thn flm. It s correspondng wth prevous reported on lterature. The Fg. 1 shows the surface morphology obtaned by SEM, whch shows a unform surface of the ZnO flms. Ths materal does not grow formng solated aggregates; t can be observed a regular dstrbuton of a knd of dsordered cylnders wth lengths between.5-1. µm. 3x1 6 x1 6 1x1 6 dn de -1x1 6 -x1 6-3x1 6-4x1 6-5x1 6 C 71 O 515 Zn 994-6x Energy (ev) Fg. 1. SEM mcrograph of our Znc Oxde Thn Flm on a glass substrate. ISSN: Issue 3, Volume 9, March 1

9 Ths materal s consdered lke photosenstve. In Fg. 11 we can see the ablty to photo detect vsble lght, but the recombnaton tme or tme to stablzaton of the materal s too large, also from the same fgure can be observed the jump of two orders of magntude n about one or two seconds. 1-4 ZnO/Glass substrate good adherence to the substrate, are homogeneous enough, and are opaque s. These ZnO flms were polycrystallne, ts crystalltes or grans have hexagonal structure, ts estmated gran sze was ~ nm, the energy gap was 3.3 ev and ts thckness was about 1 nm. The results obtaned n ths study are mportant gven ther potental mplcatons for technologcal applcatons [6-9]. I (A) Dark Lght Dark Tempo (s) Fg. 11 Photoresponse versus tme and lght condtons of our Znc Oxde Thn Flm on a glass substrate. 4 Concluson Were obtaned monolths contanng mmersed nanopartcles of ZnO and also were obtaned polycrystallne ZnO thn flms deposted on Cornng glass mcroscope sldes substrates The obtaned glasses contanng ZnO by the solgel technque were grown from TEOS as precursor, we thnk t s formed a porous or retculated vtreous matrx contanng ZnO nanopartcles n ts pores. The glasses were amorphous, wth stretchng vbraton of Zn-O and characterstc vbratons of S- O-S. So, the Raman spectrum dentfed the groups ZnO and SO. ZnO flms were obtaned by DBQ adjustng the reacton temperature to T 1 = 75 o C durng 5 mnutes and to T =85 o C durng 6 mnutes, n the same reacton, such flms are whte color, exhbt not so References: [1] Ra, H. -W.; Khan, R.; Km, J. T.; Kang, B. R.; Im, Y. H. Nanotechnology (1), 1(8), 855/1-855/5 [] Ravchandran, K.; Sakthvel, B.; Phlomnathan, Crystal Research and Technology (1), 45(3), [3] Kao, M. C.; Chen, H. Z.; Young, S. L Appled Physcs A: Materals Scence & Processng (1), 98(3), [4] Myrtl L. Kahn, Arnaud Glara, Carole Pages, Mguel Monge, Léna Sant Macary, André Masonnat and Bruno Chaudret, J. Mater. Chem., 9, 19, [5] Yamauch, Hrosh; Watanabe, Yasuyuk; Izuka, Masaak; Nakamura, Masakazu; Kudo, Kazuhro. Japanese Journal of Appled Physcs (9), 48(4, Pt. ) [6] Takahash, Hrohsa; Ishbash, Satoru. PCT Int. Appl. (9) [7] Jang, Hu; Toshma, Naok. Chemstry Letters (9), 38(6), [8] Rednger, Davd; Subramanan, Vvek, IEEE Transactons on Electron Devces (7), 54(6), [9] Iech, Hroyuk; Watanabe, Yasuyuk; Kudo, Kazuhro, Japanese Journal of Appled Physcs, (7), 46(4B), [1] Carca, P. F.; McLean, R. S.; Relly, M. H, Journal of the Socety for Informaton Dsplay (5), 13(7), [11] Cha, Sung Hoon; Oh, Mn Suk; Lee, Kwang H.; Im, Seongl; Lee, Byoung H.; Sung, Myung M. Appled Physcs Letters (8), 9(), 356/1-356/3 [1] Ohash, Naok; Kataoka, Ken; Ohgak, Takesh; Sakaguch, Isao; Haneda, Hajme, Materals Transactons (9), 5(5), [13] Park, Jong-Lo; Park, Chan; Km, Doh-Yeon; Jo, Wook; Park, Chul-Jae; Jeon, Sang-Yun; Lee, Jong-Sook. Appled Physcs Letters (9), 94(5), 518/1-518/3. ISSN: Issue 3, Volume 9, March 1

10 [14] Lany Wang,w,z,y Guoy Tang,z and Zheng- Ku Xuy J. Am. Ceram. Soc., (8), 91 [11] [15] Gurvan Brasse, Chrstne Reston, Jean- Lous Auguste, Phlppe Roy, Stephane Leparmenter, Jean-Marc Blondy, 1st WSEAS Internatonal Conference on Recent Advances n Nanotechnology Proceedngs, ISSN: , ISBN: , (9), [16] Suresh C. Plla,a John M. Kelly,*b Declan E. McCormack*c and Raghavendra Rameshd, J. Mater. Chem., 8, 18, [17] C. X. Xu and X. W. Sun Appled Physcs Letters 85, 17 [18] Adamopoulos, George; Bashr, Aneeqa; Woebkenberg, Paul H.; Bradley, Donal D. C.; Anthopoulos, Thomas D, Appled Physcs Letters (9), 95(13), 13357/ /3. [19] Brun, F. Carat, M. Casu, A. La, A. Musu, G. Pccaluga and S. Solnas Nanostruct. Mater., 1999, 11, 573. [] E. J. Kamtsos and A. P. Patss, Phys. Rev. B, 1993, 48, [1] H. Itzutzu, P. K. Har, Y. Kyozum and F. Mzwkam, Mater. Res. Bull., 1997, 3, 133. [] O. Clause, M. Kermarec, L. Bonnevot, F. Vllan and M. Che, J. Am. Chem. Soc., 199, 114, 479. [3] X. L. Xu, S. P. Lau, J. S. Chen, G. Y. Chen, B. K. Tay, J. of Crystal Growth 3 (1) 1-5. [4] N. B. Colthup, L. H. Daly, S. E. Wberley Introducton to Infrared and Raman Spectroscopy, Ac. Press (199). [5] B-M. Basol, o.m Stafsudd, A Bndal, Sola Cells, 1985, 15, [6] Ana Marja Grancarc, Anta Tarbuk, Ivancca Kovacek, 1st WSEAS Internatonal Conference on Recent Advances n Nanotechnology, ISSN: , ISBN: (9), 1-3. [7] H. Abdullah, S. Shaar, A.Amr Kadhum and M. N. Noraza, Proceedngs of the 1st WSEAS Internatonal Conference on MATERIALS SCIENCE, ISSN: , ISBN: , (8), [8] Huda Abdullah, Nugroho Pratomo Aryanto, Bran Yularto and Syarf Junad, Proceedngs of the 1st WSEAS Internatonal Conference on MATERIALS SCIENCE, ISSN: , ISBN: , (8), [9] S.J. Castllo, L.E. Regalado, M.R. Manzo-Valenca, J.C. Lopez-Cervantes, M.E. Alvarez-Ramos, A. Apolnar-Irbe and R.P. Duarte-Zamorano. New Nanotechnology Development. ISBN: (pp. 17-3). ISSN: Issue 3, Volume 9, March 1