本文選題：ZnO薄膜　切入點：電沉積　出處：《安徽大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：ZnO是具有3.37eV能隙的寬帶隙半導(dǎo)體,由于其在電子、光子和光學(xué)及生物等領(lǐng)域的出色表現(xiàn),可廣泛應(yīng)用于各類高科技領(lǐng)域。為了制備不同尺寸,晶體結(jié)構(gòu),晶形和顆粒形狀的ZnO,開發(fā)了多種制造方法。本文使用陰極電沉積法制備ZnO納米棒陣列,利用X射線衍射儀、掃描電鏡、接觸角測量儀、拉曼光譜儀等測試儀器,研究兩種基底(ITO/Ti片)上改變沉積時間、電解液組成成分比例對其微觀結(jié)構(gòu)形貌、潤濕性以及光學(xué)性能等的影響。首先,通過改變電化學(xué)沉積的時間在ITO基底上制備ZnO納米棒陣列。XRD結(jié)果表明ZnO呈六方纖鋅礦結(jié)構(gòu),隨著電沉積時間的增長,結(jié)晶度以及002方向的擇優(yōu)取向生長都得到增強,同時納米棒的直徑、表面粗糙度和ZnO納米棒陣列的厚度都變大。所有的樣品都展現(xiàn)出疏水性,水接觸角在電沉積120min時逐漸上升到120°,經(jīng)過10min紫外光照,ZnO納米棒陣列表面潤濕性轉(zhuǎn)化為親水性,光照后水接觸角與未經(jīng)紫外照射前的比例為73.5%、63.5%、48.3%和24.2%,分別對應(yīng)沉積時間10min、30min、60min和120min的樣品。光致發(fā)光(PL)光譜結(jié)果顯示隨著電沉積時間的增加,ZnO的紫外發(fā)光峰(本征發(fā)光峰)的峰強比由2.26%提升到63.84%,同時可見光發(fā)光峰(缺陷導(dǎo)致的發(fā)光峰)的峰強比降低,說明沉積時間從10min增長至120min,ZnO薄膜的內(nèi)在缺陷減少。拉曼圖譜的分析表明,ZnO納米棒陣列在這些條件下呈現(xiàn)439cm-1,566cm-1,和1097cm-1三處特征峰,分別對應(yīng)了ZnO陣列的E2光聲子振動模、EIL光聲子振動模以及E3單晶振動模。隨后,保持其他條件不變,改變電解液濃度組成(Zn2+濃度不變),在Zn(N03)2中摻入ZnCl2溶液,XRD結(jié)果表明,所有的峰都歸因于六方纖鋅礦結(jié)構(gòu),晶粒尺寸隨著ZnCl2濃度的增加而變小,晶核數(shù)量增加,同時c軸(002)方向擇優(yōu)取向減弱。SEM結(jié)果顯示,隨著Zn(NO3)2濃度的降低,納米結(jié)構(gòu)由棒狀變?yōu)殄F狀,其中ZnO的直徑,除了濃度比為1:1的樣品之外,持續(xù)減小,且納米結(jié)構(gòu)的頂端由"吞并"狀態(tài)改變?yōu)檫h離,間隙得到增加。PL光譜顯示Zn(NO3)2電解液制備的樣品A紫外發(fā)射峰相對較強,隨著電解液中ZnCl2濃度比的增加,紫外發(fā)射峰比率增強,純ZnCl2電解液制備的樣品E的紫外發(fā)射峰比率為最小,缺陷最多,隨著氯離子濃度的增大,一個極少見的位于350nm處的發(fā)光峰逐漸顯現(xiàn)。在紫外照射之前所有的樣品均表現(xiàn)為較強的疏水性,且隨著ZnC12濃度的增長,水接觸角有先增加后減小的趨勢,可能與表面粗糙度變大以及結(jié)晶度變差的綜合結(jié)果有關(guān)。ZnO納米棒陣列的可潤濕性在15分鐘紫外照射后從疏水性改變?yōu)橛H水性,并且水接觸角的光誘導(dǎo)變化從45 8至12.9%,這可能是與潤濕模型的變化、ZnO納米結(jié)構(gòu)的表面粗糙度大小差異以及間隙有關(guān)。紫外吸收譜表明,隨電解液中氯離子濃度的增加而增加,禁帶寬度不斷增加至3.34接近標(biāo)準(zhǔn)值3.37eV。最后,改變沉積時間在Ti片上制備ZnO納米棒陣列。SEM結(jié)果顯示,所有樣品均為棒狀六棱錐形貌,隨著電沉積時間的增加,納米棒的直徑、棒之間的間隙減小。在PL光譜中所有樣品都具有窄的紫外發(fā)射峰,在可見光區(qū)顯示寬的發(fā)光區(qū),并且隨著電沉積時間增加,缺陷先減小后增加,在45 min時候達到最小。樣品的沉積時間由15分鐘增長到60分鐘,在紫外照射之前的水接觸角逐漸變小,這可能與表面粗糙度變小有關(guān)。ZnO納米棒陣列的可潤濕性在2小時紫外照射后全部轉(zhuǎn)換為超親水性,并且水接觸角還原率的光誘導(dǎo)變化先變大后變小,在45 min時達到最大,這可能與潤濕模型的轉(zhuǎn)變、ZnO納米棒陣列的表面粗糙度大小差異以及薄膜的缺陷多少有關(guān)。禁帶寬度曲線與光電流曲線都與PL光譜有相同的規(guī)律性,都在45 min時候達到最大值(紫外峰強、禁帶寬度與光電流大小)。
[Abstract]:ZnO is a wide band gap semiconductor 3.37eV gap, because of its excellent performance in electronic, photonic and optical and biological fields, can be widely used in all kinds of high-tech fields. In order to prepare different sizes, crystal structure, morphology and particle shape of ZnO, the development of a variety of manufacturing methods. This paper use cathodic electrodeposition ZnO nanorod array, using X ray diffraction, scanning electron microscopy, contact angle measurements, Raman spectrometer, research on two kinds of substrate (ITO/Ti) on the deposition time, electrolyte composition on the microstructure morphology composition, wettability and optical properties. Firstly, by changing the electrochemical deposition time in the ITO substrate to prepare ZnO nanorod array.XRD results show that ZnO is the six wurtzite structure with the deposition time increases, the crystallinity and the 002 direction of the preferred orientation growth have been enhanced At the same time, the diameter of the nanorods, surface roughness and thickness of ZnO nanorod arrays have become large. All the samples exhibit hydrophobicity, the water contact angle in the electrodeposition of 120min gradually increased to 120 DEG 10min after UV irradiation, ZnO nanorod arrays of surface wetting into hydrophilic, light water contact angle 63.5% and without UV irradiation before the ratio of 73.5%, 48.3% and 24.2% respectively, the corresponding deposition time of 10min, 30min, 60min and 120min samples. The photoluminescence (PL) spectroscopy results show that with the increasing of deposition time, ZnO ultraviolet emission peak (intrinsic emission peak) by the peak intensity ratio 2.26% to 63.84%, while the visible emission peak (peak of defects) that peak intensity ratio decreased, the deposition time increased from 10min to 120min, reduce the internal defects of ZnO thin films. The Raman spectrum analysis showed that ZnO nanorod arrays show 439cm-1 under these conditions 566cm-1, 1097cm-1, and three peaks, corresponding to the E2 optical phonon vibration mode ZnO array, EIL optical phonon vibration mode and vibration mode of E3 single crystal. Then, keeping other conditions unchanged, changes in the composition of the electrolyte concentration (the concentration of Zn2+, Zn in the same) (N03) 2 doped ZnCl2 solution, XRD results show that, all peaks are attributed to six wurtzite structure. The grain size increases with the concentration of ZnCl2 decreases, the nucleation number increased, while the c axis (002) direction orientation weakened.SEM results showed that with Zn (NO3) to reduce the concentration of 2, nano structure by rods is conical. The diameter of ZnO, in addition, the concentration ratio of 1:1 sample decreased continuously, and the top of nano structure by the "annex" state changes from, clearance increased.PL spectra show that Zn (NO3) 2 electrolyte samples prepared by A UV emission peak phase of strong, with the increase of the ratio of ZnCl2 concentration in electrolyte And the UV emission ratio enhanced UV E pure ZnCl2 sample preparation of the electrolyte the emission peak ratio is the smallest, most defects, with the increase of the concentration of chloride ion, a rare peak is located at 350nm gradually. Before UV irradiation all samples showed strong hydrophobicity and with the concentration of ZnC12 increased, the water contact angle is increased first and then decreased, the comprehensive result may be related to surface roughness becomes larger and the poor crystallinity of.ZnO nanorod array wettability in 15 minutes after UV irradiation from hydrophobic to hydrophilic change, and the water contact angle of light induced changes from 458 to 12.9%, this may be the change and wetting model, the surface roughness of ZnO nano structure size difference and gap. The UV absorption spectra showed that increased with the increase of the concentration of chloride ion in the electrolyte, the band gap is increasing To 3.34 close to the standard value of 3.37eV. finally, the deposition time on Ti wafer fabrication of ZnO nanorod array.SEM results showed that all the samples were respectively six pyramid morphology, with the increase of deposition time, the diameter of the nanorods, the gap between the bars decreases. In the PL spectra of all samples have narrow UV emission peaks in the visible region display light emitting region wide, and with the deposition time increased, the defect decreases first and then increases and reaches the minimum at 45 min. When the deposition time of samples from 15 minutes to 60 minutes, the contact angle of growth, gradually decreased before UV irradiation of water, which may be related to the surface roughness is smaller the wettability of the.ZnO nanorod arrays in 2 hours after UV irradiation converted into super hydrophilic and water contact angle reduction rate of light induced changes at first then decreased, reached the maximum at 45 min, this may change with the wetting model The surface roughness of ZnO nanorod arrays is related to the size difference and the defect of the films. The forbidden band width curves and photocurrent curves have the same regularity as those of PL spectra. They reach the maximum value at 45 min (ultraviolet peak intensity, band gap and photocurrent size).

【學(xué)位授予單位】：安徽大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O614.241;TB383.1

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