脉冲激光沉积ZnO薄膜及其性质研究
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摘要
氧化锌(ZnO)是一种纤锌矿结构的宽带隙Ⅱ-Ⅵ族化合物半导体材料,室温下的禁带宽度约为3.37eV,激子结合能高达60meV,具有优异的光学和电学性能,在透明导电薄膜、表面声波器件、气体传感器和光电器件等方面有着广泛的应用,特别是高质量ZnO薄膜室温紫外受激发射的实现,使其成为紫外激光的重要材料,因此对氧化锌的研究已成为继GaN之后宽带隙半导体研究的又一热点。本文围绕飞秒脉冲激光沉积(fsPLD)法制备高质量ZnO/Si薄膜而展开研究工作。
首先综述了ZnO薄膜的制备方法及国内外研究状况,分析了fsPLD法制备ZnO薄膜的特点,提出了一种以fsPLD法制备大面积均匀ZnO/Si薄膜的方法。
其次,详细研究了fsPLD法制备薄膜的过程中工艺参数(如衬底温度、脉冲激光能量、环境氧气压强等)及退火处理对薄膜质量的影响,并与纳秒脉冲激光沉积(nsPLD)法制备的薄膜进行比较。采用X射线衍射(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(ATM)、可见-紫外(UV-Vis)透射谱、傅里叶变换红外谱(FTIR)、光致发光谱(PL)等对薄膜的结构、形貌特征及光学性能进行表征,得到一系列新结果。
首次在较低的衬底温度(80℃)下,以fsPLD法制备出高c-轴取向的薄膜;薄膜的c-轴取向度、晶面间距及可见光透过率在80℃时达到最大值;薄膜的晶粒度随着衬底温度的升高而增加;退火后薄膜的取向性变化不大、晶面间距缩小、晶粒度变大,且不同温度下生长的薄膜退火后晶粒度趋于相等。首次在较低的氧压(2.0mPa)下,以fsPLD法制备出发光性能优良的薄膜;ZnO薄膜的光致发光谱主要有紫外发射带和可见光发射带,紫外发射是ZnO的本征发射,可见光发射与缺陷和杂质有关;当氧压低于1.0mPa时,薄膜除了具有382nm的紫外发射峰外,还存在很强的410nm的紫光发射峰,当氧压增至2.0mPa时,可见光发射带变得微弱,当氧压增至5.0mPa时,可见光发射带完全消失,只剩下唯一强而狭窄的376nm的紫外发射峰,表明可见光发射与氧空位有关。首次报导通过提高激光能量可使制备的薄膜晶粒细化而致密,且薄膜的晶粒度与发光性能有关。所制备的薄膜在空气中退火后可见光透过率提高,FTIR谱Zn-O键吸收峰变强变窄,PL光谱紫外发射峰变弱。与nsPLD法相比,fsPLD法所制备的薄膜晶粒更为细小致密、表面更为光滑、具有更高的可见光透过率和更强更窄的PL紫外发射峰。
Zinc oxide(ZnO) is a kind ofⅡ-Ⅵwide band gap compound semiconductor of wurtzite structure with a direct band gap of 3.37 eV at room temperature,exciton binding energy of 60 meV,which makes it have many applications,such as transparent conducting films,surface acoustic wave devices,gas sensors and photo-electronic devices.The report of ultraviolet laser emission of high quality ZnO thin films at room temperature attracted a lot of attention in ZnO researching.Like GaN compound,the research about ZnO has burned white hot in the range of wide band gap.The high quality ZnO thin films deposited by femtosecond pulsed laser deposition(fsPLD) on Si substrates were investigated in this dissertation.
First,the progress of preparation techniques for ZnO thin films was summarized,the characteristics of the ZnO films deposited by fsPLD was analyzed,and a method to deposit large area ZnO thin films was provided.
Second,the effects of technology parameters,such as substrate temperature,single pulsed laser energy,oxygen pressure and annealing on the quality of ZnO thin films deposited by fsPLD were studied in detail.The differences of the ZnO thin films deposited by fsPLD and nanosecond pulsed laser deposition(nsPLD) were investigated.The structural properties of the thin films were analyzed by x-ray diffraction(XRD).The surface morphologies of the films were observed by field scan electron microscope (FESEM) and atom force microscope(AFM).The optical properties of the thin films were investigated by ultraviolet-visible(UV-vis) spectra,Fourier-transform infrared(FTIR) spectra and photoluminescence(PL) spectra.A series of new results were obtained.
Highly c-axis orientation degrees of ZnO thin films were obtained on lower substrate temperature(80℃) deposited by fsPLD for the first time.The c-axis orientation degrees, (002) spacing,and the visible transmittances reached the max at 80℃.The mean grain size of the films increased with the increasing of substrate temperature.The(002) spacing decreased and the orientation degrees had no changes after annealing.The mean grain size deposited at different temperature increased and reached to the same size after annealing. Highly efficient luminescent ZnO thin films were prepared at lower oxygen pressure(2.0 mPa) deposited by fsPLD.The PL spectra of ZnO films mainly contain the UV emission band and the visible emission band.The UV emission band is due to the near band-edge emission,and the visible emission band is result in impurities or defects.The films contained UV emission peak at wavelength of 382 nm and violet emission peak at 410 nm growth below oxygen pressure 1.0 mPa.The violet emission peak of 410 nm disappeared while the oxygen pressure increasing to 2.0 mPa and the visible emission band become very weak at the same time.The visible emission band disappeared completely with the oxygen pressure increasing to 5.0mPa,and only a narrower and stronger UV emission peak was in existence at 376 nm.It indicated that the visible emission band was resulted from oxygen vacancy.By increasing the pulsed laser energy,we could obtain the smaller and denser crystalline ZnO films,which is helpful for the UV emission.After annealing in the air at 600℃for 10 hours,the transmittances of the ZnO films increased,and the Zn-O absorption peak in the FTIR spectra became narrower and stronger.Comparing with nsPLD method,the ZnO thin films deposited by nsPLD had smaller craystallinity,a smoother surface,higher visible transmitances in UV-vis spectra and narrower UV emission peak at 376 nm in PL spectra.
首先综述了ZnO薄膜的制备方法及国内外研究状况,分析了fsPLD法制备ZnO薄膜的特点,提出了一种以fsPLD法制备大面积均匀ZnO/Si薄膜的方法。
其次,详细研究了fsPLD法制备薄膜的过程中工艺参数(如衬底温度、脉冲激光能量、环境氧气压强等)及退火处理对薄膜质量的影响,并与纳秒脉冲激光沉积(nsPLD)法制备的薄膜进行比较。采用X射线衍射(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(ATM)、可见-紫外(UV-Vis)透射谱、傅里叶变换红外谱(FTIR)、光致发光谱(PL)等对薄膜的结构、形貌特征及光学性能进行表征,得到一系列新结果。
首次在较低的衬底温度(80℃)下,以fsPLD法制备出高c-轴取向的薄膜;薄膜的c-轴取向度、晶面间距及可见光透过率在80℃时达到最大值;薄膜的晶粒度随着衬底温度的升高而增加;退火后薄膜的取向性变化不大、晶面间距缩小、晶粒度变大,且不同温度下生长的薄膜退火后晶粒度趋于相等。首次在较低的氧压(2.0mPa)下,以fsPLD法制备出发光性能优良的薄膜;ZnO薄膜的光致发光谱主要有紫外发射带和可见光发射带,紫外发射是ZnO的本征发射,可见光发射与缺陷和杂质有关;当氧压低于1.0mPa时,薄膜除了具有382nm的紫外发射峰外,还存在很强的410nm的紫光发射峰,当氧压增至2.0mPa时,可见光发射带变得微弱,当氧压增至5.0mPa时,可见光发射带完全消失,只剩下唯一强而狭窄的376nm的紫外发射峰,表明可见光发射与氧空位有关。首次报导通过提高激光能量可使制备的薄膜晶粒细化而致密,且薄膜的晶粒度与发光性能有关。所制备的薄膜在空气中退火后可见光透过率提高,FTIR谱Zn-O键吸收峰变强变窄,PL光谱紫外发射峰变弱。与nsPLD法相比,fsPLD法所制备的薄膜晶粒更为细小致密、表面更为光滑、具有更高的可见光透过率和更强更窄的PL紫外发射峰。
Zinc oxide(ZnO) is a kind ofⅡ-Ⅵwide band gap compound semiconductor of wurtzite structure with a direct band gap of 3.37 eV at room temperature,exciton binding energy of 60 meV,which makes it have many applications,such as transparent conducting films,surface acoustic wave devices,gas sensors and photo-electronic devices.The report of ultraviolet laser emission of high quality ZnO thin films at room temperature attracted a lot of attention in ZnO researching.Like GaN compound,the research about ZnO has burned white hot in the range of wide band gap.The high quality ZnO thin films deposited by femtosecond pulsed laser deposition(fsPLD) on Si substrates were investigated in this dissertation.
First,the progress of preparation techniques for ZnO thin films was summarized,the characteristics of the ZnO films deposited by fsPLD was analyzed,and a method to deposit large area ZnO thin films was provided.
Second,the effects of technology parameters,such as substrate temperature,single pulsed laser energy,oxygen pressure and annealing on the quality of ZnO thin films deposited by fsPLD were studied in detail.The differences of the ZnO thin films deposited by fsPLD and nanosecond pulsed laser deposition(nsPLD) were investigated.The structural properties of the thin films were analyzed by x-ray diffraction(XRD).The surface morphologies of the films were observed by field scan electron microscope (FESEM) and atom force microscope(AFM).The optical properties of the thin films were investigated by ultraviolet-visible(UV-vis) spectra,Fourier-transform infrared(FTIR) spectra and photoluminescence(PL) spectra.A series of new results were obtained.
Highly c-axis orientation degrees of ZnO thin films were obtained on lower substrate temperature(80℃) deposited by fsPLD for the first time.The c-axis orientation degrees, (002) spacing,and the visible transmittances reached the max at 80℃.The mean grain size of the films increased with the increasing of substrate temperature.The(002) spacing decreased and the orientation degrees had no changes after annealing.The mean grain size deposited at different temperature increased and reached to the same size after annealing. Highly efficient luminescent ZnO thin films were prepared at lower oxygen pressure(2.0 mPa) deposited by fsPLD.The PL spectra of ZnO films mainly contain the UV emission band and the visible emission band.The UV emission band is due to the near band-edge emission,and the visible emission band is result in impurities or defects.The films contained UV emission peak at wavelength of 382 nm and violet emission peak at 410 nm growth below oxygen pressure 1.0 mPa.The violet emission peak of 410 nm disappeared while the oxygen pressure increasing to 2.0 mPa and the visible emission band become very weak at the same time.The visible emission band disappeared completely with the oxygen pressure increasing to 5.0mPa,and only a narrower and stronger UV emission peak was in existence at 376 nm.It indicated that the visible emission band was resulted from oxygen vacancy.By increasing the pulsed laser energy,we could obtain the smaller and denser crystalline ZnO films,which is helpful for the UV emission.After annealing in the air at 600℃for 10 hours,the transmittances of the ZnO films increased,and the Zn-O absorption peak in the FTIR spectra became narrower and stronger.Comparing with nsPLD method,the ZnO thin films deposited by nsPLD had smaller craystallinity,a smoother surface,higher visible transmitances in UV-vis spectra and narrower UV emission peak at 376 nm in PL spectra.
引文
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