ZnO纳米结构与器件的制备和研究
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摘要
近年来,半导体纳米结构因其在先进器件等方面存在广阔的应用前景,而成为国内外纳米领域人们关注的热点。其中,ZnO纳米阵列结构被认为是最具有应用前景的纳米材料之一。ZnO是一种宽禁带直接带隙Ⅱ-Ⅳ族半导体材料,室温下禁带宽度为3.37 eV,具有较大的激子束缚能(60 meV),是制备下一代短波长发光二极管(LED)和激光器的最佳候选者之一;它具有良好的压电性和生物适合性,可用于压电传感器、机电耦合传感器、表面声波器件、微机电系统和生物医药等领域。而且,制备ZnO纳米结构的技术较多,如:化学气相沉积(CVD)、金属有机化学气相沉积(MOCVD)、热蒸发、分子束外延(MBE)等。因此,ZnO纳米结构成为众多研究者关注的焦点,许多研究人员通过各种制备技术得到了不同形貌和性质的ZnO纳米结构。本文以ZnO材料为出发点,重点研究了目前阻碍ZnO基纳米器件发展的难点问题:制备高质量的ZnO纳米结构阵列和p型掺杂ZnO纳米结构。同时对ZnO基纳米线场效应晶体管器件进行了初步研究。
通常人们采用金属催化的方法生长ZnO纳米结构,但是这些金属催化剂会引入新的杂质缺陷,所以发展无催化方法制备ZnO纳米结构是很有必要的。据了解,到目前为止还没有关于无金属催化的脉冲激光沉积(PLD)方法制备ZnO纳米结构的报道。本文采用PLD技术通过独特的方法在InP衬底上实现了ZnO纳米结构阵列的可控生长,实验中没有采用金属催化剂,避免引入了新的杂质缺陷。通过SEM、XRD、PL谱等表征手段对其进行了表征,结果表明制备出的ZnO纳米结构具有较好的表面形貌和结晶质量,常温PL呈现出紫外发射峰和绿光发射峰,表现出良好的光学性质。这种简单的PLD法为进一步制备质量满足纳米器件要求的ZnO纳米结构提供了一种无金属催化的生长方法。
进一步优化生长条件制备出整齐的ZnO纳米结构阵列。SEM显示制备出的ZnO纳米结构阵列具有很好的表面形貌和择优生长取向;XRD测试结果表明ZnO纳米结构阵列结晶质量很好;低温PL谱出现新奇的现象,通过比较不同生长温度的低温PL谱,推断磷元素可以从InP衬底溢出扩散进入ZnO,形成磷掺杂的ZnO(ZnO:P)纳米结构阵列;采用变温和变激发PL光谱对光学特性和发光机理进行了细致研究,证实了磷元素是作为受主掺杂进入ZnO纳米结构阵列;采用Arrhenius公式对实验数据进行拟合计算,计算出的受主束缚能E_A的数值与理论模型预言和其他课题组得到的实验数据相符合。本实验成功制备出ZnO:P纳米结构阵列,为实现ZnO基纳米器件的p型掺杂提供了一种可借鉴的方法。
通过在反应源中加入P_2O_5粉末的简单约束管化学气相沉积方法在α-蓝宝石衬底上制备出具有奇特形貌的磷掺杂ZnO纳米四角棱锥结构。SEM测试显示未掺杂和磷掺杂的ZnO纳米四角棱锥结构具有相似的形貌特征,但是ZnO:P纳米四角棱锥的顶端要比未掺杂的尖锐;XRD测试结果表明制备出的未掺杂和磷掺杂的ZnO纳米四角棱锥具有良好的晶体质量;选择区域电子衍射出现了清晰的矩形亮斑衍射花样说明未掺杂和磷掺杂的ZnO纳米四角棱锥的晶体结构为六角纤锌矿结构,结晶质量很好具有明显的(002)择优生长取向;通过比较未掺杂和磷掺杂样品的低温PL谱,发现未掺杂样品出现施主束缚激子(D~0X)和自由激子相关的发射峰,磷掺杂样品的低温PL谱中D~0X消失并出现了几个新的发射峰,推测这几个发射峰应该是与磷掺杂有关,采用变温和变激发PL谱表征磷掺杂样品的光学性质,通过对机理的分析确认这几个发射峰是与磷受主掺杂相关的:A~0X,FA,DAP以及DAP-1LO,因此证实了磷元素是作为受主掺杂进入ZnO。利用Arrhenius公式和Haynes规则通过实验数据拟合得出受主束缚能E_A。本实验通过一种简单的CVD方法和一种廉价的P_2O_5掺杂源实现了ZnO纳米结构的p型掺杂,这为进一步实现ZnO基纳米器件提供了一种可行的p型掺杂方法。
通过化学气相沉积方法生长出ZnO纳米线,利用电子束蒸发和光刻技术制备出规则的微米级Au电极,将单根ZnO纳米线搭连在Au电极上,组装出了最基本的半导体ZnO纳米线场效应晶体管。利用Ⅰ-Ⅴ特性测试仪对制作的ZnO纳米线场效应晶体管的Ⅰ-Ⅴ特性进行测试分析,结果显示该场效应晶体管具有良好的整流特性,达到了场效应晶体管应用的基本要求。
Zinc oxide(ZnO) is a unique semiconductor material with a wide direct band gap of 3.37 eV and a relatively large exciton binding energy of 60 meV at room temperature.In recent year,it has attracted increasing interests.It has been regarded as one of the most promising candidates for the next generation of short-wavelength light emitting diode(LED) and laser devices.With the development of nanoscience and nanotechnology,semiconductor nanomaterials will have great influences not only in the fields of physics,chemistry,biology and material science,but also in medicine and information technology.The availability of a rich genre of nanostructures makes ZnO an ideal material for nanoscale optoelectronics devices in the visible and near ultraviolet regions.Furthermore,functional devices such as nanostructure field-effect transistors(FETs),electromechanical coupled sensor,piezoelectric nanosensors,surface acoustic wave(SAW) device,micro-electro mechanical systems (MEMS) and nanolasers have already been realized.Moreover,since ZnO is a biocompatible material,ZnO nanomaterials are expected to be used for biochemical,biomedical,and biomolecular applications.In addition,various techniques are employed to fabricate ZnO nanostructures,such as chemical vapor deposition(CVD),metal-organic chemical vapor deposition(MOCVD),thermal evaporation,molecule beam epitaxy(MBE),etc.Therefore, ZnO nanostructures have attracted so much attention,and a large number of publications have been presented recently for reporting ZnO nanostrucmres with diverse morphologies and properties grown by different approaches.In order to develop nano-scale devices based on ZnO,fabrication high quality ZnO nanostructure arrays and p-type ZnO nanostructures are essential.
The assistance of metal catalysts is the most widely used technique for synthesis aligned ZnO nanostrucmres.However.metal catalysts commonly introduce extra impurities defects in the products.Consequently.it is necessary to develop catalyst-free growth techniques of ZnO nanostructures.As we known,there is no report about catalyst-free preparing ZnO nanostructures by pulse laser deposition(PLD) technique.In this thesis,ZnO nanonod arrays were deposited on InP(001) wafer by PLD system with a KrF excimer laser.ZnO seed-layer and buffer-layer rather than metal was used as the catalyst for fabricating ZnO nanostructure. The synthesized ZnO nanorod arrays exhibited a strong c-axis preferential growth orientation with high crystalline quality,and well optical quality.It reveals that the method is a effective technique for growing ZnO nanostructures without metal catalysts.The well aligned and separated ZnO nanorods fabricated by this comparatively simple technique sheds light on further applications for nano-devices.
ZnO is naturally an n-type materials,p-type doping is still a bottleneck to device fabrication.Both theoretical model and experimental results illustrate that phosphorus element may act as effective p-type dopants for ZnO thin films.As for the development of ZnO:P nanostructures,very few reports have been published thus far.In this thesis,ZnO:P nanorods and nanoneedles were successfully synthesized by phosphorus diffusion from an InP substrate using a PLD technique.Low temperature(10 K) PL spectra near-band-edge emission peaks were attributed to acceptor-related A~0X,FA,and DAP transitions.The effect of p-doping on the optical characteristics of the ZnO nanorods was investigated by excitation intensity and temperature dependent PL spectra.Morover,the value of the acceptor energy level of the phosphorus dopant,determined by experimental data and fitting,agree well with the corresponding theoretical and experimental values in ZnO:P films and nanowires.
Although p-type ZnO thin films have been reported by some research groups,the availability of p-type doping ZnO nanostructure is very scarce.The Lack of p-type ZnO nanostructure is currently the major factor precluding the realization of a wide range of functional nanodevices based on ZnO.High-quality novel undoped and phosphorus-doped ZnO nanotetrapods were synthesized on sapphire substrates by a simple chemical vapor deposition(CVD) method.Phosphorus doping was performed by using P_2O_5 as the dopant source.Low temperature PL spectrum exhibited acceptor related emission peaks.P-type doping signals were confirmed by temperature and excitation intensity dependent PL measurements.X-ray diffraction and selected area electron diffraction results revealed that crystalline quality and structure of ZnO single crystals were not degraded by phosphorus doping.The binding energy of phosphorus acceptor dopant was established to be about 120 meV.The synthesis of p-type doping ZnO nanotetrapods sheds light on further applications for nanolasers,nanosensors,biocompatible materials etc..and opens up enormous opportunities for nanoscale electronics,optoelectronics and biologics.
The simple ZnO nanowire-based field effect transistor(FET) was fabricated by linking up a ZnO nanowire with two Au electrodes,where ZnO nanowires were synthesized by chemical physics deposition,Au electrodes were fabricated using photolithography and electron beam evaporation technologies.The current-voltage results presented favorableⅠ-Ⅴcharacteristics curves.
通常人们采用金属催化的方法生长ZnO纳米结构,但是这些金属催化剂会引入新的杂质缺陷,所以发展无催化方法制备ZnO纳米结构是很有必要的。据了解,到目前为止还没有关于无金属催化的脉冲激光沉积(PLD)方法制备ZnO纳米结构的报道。本文采用PLD技术通过独特的方法在InP衬底上实现了ZnO纳米结构阵列的可控生长,实验中没有采用金属催化剂,避免引入了新的杂质缺陷。通过SEM、XRD、PL谱等表征手段对其进行了表征,结果表明制备出的ZnO纳米结构具有较好的表面形貌和结晶质量,常温PL呈现出紫外发射峰和绿光发射峰,表现出良好的光学性质。这种简单的PLD法为进一步制备质量满足纳米器件要求的ZnO纳米结构提供了一种无金属催化的生长方法。
进一步优化生长条件制备出整齐的ZnO纳米结构阵列。SEM显示制备出的ZnO纳米结构阵列具有很好的表面形貌和择优生长取向;XRD测试结果表明ZnO纳米结构阵列结晶质量很好;低温PL谱出现新奇的现象,通过比较不同生长温度的低温PL谱,推断磷元素可以从InP衬底溢出扩散进入ZnO,形成磷掺杂的ZnO(ZnO:P)纳米结构阵列;采用变温和变激发PL光谱对光学特性和发光机理进行了细致研究,证实了磷元素是作为受主掺杂进入ZnO纳米结构阵列;采用Arrhenius公式对实验数据进行拟合计算,计算出的受主束缚能E_A的数值与理论模型预言和其他课题组得到的实验数据相符合。本实验成功制备出ZnO:P纳米结构阵列,为实现ZnO基纳米器件的p型掺杂提供了一种可借鉴的方法。
通过在反应源中加入P_2O_5粉末的简单约束管化学气相沉积方法在α-蓝宝石衬底上制备出具有奇特形貌的磷掺杂ZnO纳米四角棱锥结构。SEM测试显示未掺杂和磷掺杂的ZnO纳米四角棱锥结构具有相似的形貌特征,但是ZnO:P纳米四角棱锥的顶端要比未掺杂的尖锐;XRD测试结果表明制备出的未掺杂和磷掺杂的ZnO纳米四角棱锥具有良好的晶体质量;选择区域电子衍射出现了清晰的矩形亮斑衍射花样说明未掺杂和磷掺杂的ZnO纳米四角棱锥的晶体结构为六角纤锌矿结构,结晶质量很好具有明显的(002)择优生长取向;通过比较未掺杂和磷掺杂样品的低温PL谱,发现未掺杂样品出现施主束缚激子(D~0X)和自由激子相关的发射峰,磷掺杂样品的低温PL谱中D~0X消失并出现了几个新的发射峰,推测这几个发射峰应该是与磷掺杂有关,采用变温和变激发PL谱表征磷掺杂样品的光学性质,通过对机理的分析确认这几个发射峰是与磷受主掺杂相关的:A~0X,FA,DAP以及DAP-1LO,因此证实了磷元素是作为受主掺杂进入ZnO。利用Arrhenius公式和Haynes规则通过实验数据拟合得出受主束缚能E_A。本实验通过一种简单的CVD方法和一种廉价的P_2O_5掺杂源实现了ZnO纳米结构的p型掺杂,这为进一步实现ZnO基纳米器件提供了一种可行的p型掺杂方法。
通过化学气相沉积方法生长出ZnO纳米线,利用电子束蒸发和光刻技术制备出规则的微米级Au电极,将单根ZnO纳米线搭连在Au电极上,组装出了最基本的半导体ZnO纳米线场效应晶体管。利用Ⅰ-Ⅴ特性测试仪对制作的ZnO纳米线场效应晶体管的Ⅰ-Ⅴ特性进行测试分析,结果显示该场效应晶体管具有良好的整流特性,达到了场效应晶体管应用的基本要求。
Zinc oxide(ZnO) is a unique semiconductor material with a wide direct band gap of 3.37 eV and a relatively large exciton binding energy of 60 meV at room temperature.In recent year,it has attracted increasing interests.It has been regarded as one of the most promising candidates for the next generation of short-wavelength light emitting diode(LED) and laser devices.With the development of nanoscience and nanotechnology,semiconductor nanomaterials will have great influences not only in the fields of physics,chemistry,biology and material science,but also in medicine and information technology.The availability of a rich genre of nanostructures makes ZnO an ideal material for nanoscale optoelectronics devices in the visible and near ultraviolet regions.Furthermore,functional devices such as nanostructure field-effect transistors(FETs),electromechanical coupled sensor,piezoelectric nanosensors,surface acoustic wave(SAW) device,micro-electro mechanical systems (MEMS) and nanolasers have already been realized.Moreover,since ZnO is a biocompatible material,ZnO nanomaterials are expected to be used for biochemical,biomedical,and biomolecular applications.In addition,various techniques are employed to fabricate ZnO nanostructures,such as chemical vapor deposition(CVD),metal-organic chemical vapor deposition(MOCVD),thermal evaporation,molecule beam epitaxy(MBE),etc.Therefore, ZnO nanostructures have attracted so much attention,and a large number of publications have been presented recently for reporting ZnO nanostrucmres with diverse morphologies and properties grown by different approaches.In order to develop nano-scale devices based on ZnO,fabrication high quality ZnO nanostructure arrays and p-type ZnO nanostructures are essential.
The assistance of metal catalysts is the most widely used technique for synthesis aligned ZnO nanostrucmres.However.metal catalysts commonly introduce extra impurities defects in the products.Consequently.it is necessary to develop catalyst-free growth techniques of ZnO nanostructures.As we known,there is no report about catalyst-free preparing ZnO nanostructures by pulse laser deposition(PLD) technique.In this thesis,ZnO nanonod arrays were deposited on InP(001) wafer by PLD system with a KrF excimer laser.ZnO seed-layer and buffer-layer rather than metal was used as the catalyst for fabricating ZnO nanostructure. The synthesized ZnO nanorod arrays exhibited a strong c-axis preferential growth orientation with high crystalline quality,and well optical quality.It reveals that the method is a effective technique for growing ZnO nanostructures without metal catalysts.The well aligned and separated ZnO nanorods fabricated by this comparatively simple technique sheds light on further applications for nano-devices.
ZnO is naturally an n-type materials,p-type doping is still a bottleneck to device fabrication.Both theoretical model and experimental results illustrate that phosphorus element may act as effective p-type dopants for ZnO thin films.As for the development of ZnO:P nanostructures,very few reports have been published thus far.In this thesis,ZnO:P nanorods and nanoneedles were successfully synthesized by phosphorus diffusion from an InP substrate using a PLD technique.Low temperature(10 K) PL spectra near-band-edge emission peaks were attributed to acceptor-related A~0X,FA,and DAP transitions.The effect of p-doping on the optical characteristics of the ZnO nanorods was investigated by excitation intensity and temperature dependent PL spectra.Morover,the value of the acceptor energy level of the phosphorus dopant,determined by experimental data and fitting,agree well with the corresponding theoretical and experimental values in ZnO:P films and nanowires.
Although p-type ZnO thin films have been reported by some research groups,the availability of p-type doping ZnO nanostructure is very scarce.The Lack of p-type ZnO nanostructure is currently the major factor precluding the realization of a wide range of functional nanodevices based on ZnO.High-quality novel undoped and phosphorus-doped ZnO nanotetrapods were synthesized on sapphire substrates by a simple chemical vapor deposition(CVD) method.Phosphorus doping was performed by using P_2O_5 as the dopant source.Low temperature PL spectrum exhibited acceptor related emission peaks.P-type doping signals were confirmed by temperature and excitation intensity dependent PL measurements.X-ray diffraction and selected area electron diffraction results revealed that crystalline quality and structure of ZnO single crystals were not degraded by phosphorus doping.The binding energy of phosphorus acceptor dopant was established to be about 120 meV.The synthesis of p-type doping ZnO nanotetrapods sheds light on further applications for nanolasers,nanosensors,biocompatible materials etc..and opens up enormous opportunities for nanoscale electronics,optoelectronics and biologics.
The simple ZnO nanowire-based field effect transistor(FET) was fabricated by linking up a ZnO nanowire with two Au electrodes,where ZnO nanowires were synthesized by chemical physics deposition,Au electrodes were fabricated using photolithography and electron beam evaporation technologies.The current-voltage results presented favorableⅠ-Ⅴcharacteristics curves.
引文
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