铕掺杂富硅氧化硅薄膜的光电性能研究
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摘要
硅基光源是硅基光电子的重要组成部分,也是硅基光电子发展所面临的首要问题之一,但由于晶体硅的间接带隙特性,使得其不适合应用于光学有源器件中。稀土离子,由于具有荧光强度高,单色性好,性能稳定等特性而受到广泛关注。因而硅基稀土发光器件有可能用于硅基光电子所需光源。本文就稀土铕掺杂的富硅氧化硅薄膜的光学和电学性能进行研究,探索其作为硅基光源的途径。
铕掺杂的富硅氧化硅薄膜是通过电子束蒸发法(EBE)进行制备,铕的掺杂剂量是通过蒸发源中的掺杂剂量进行控制。通过对薄膜制备条件以及后续热处理过程与发光特性(PL)间的关系进行了详细研究,并将薄膜制备成MOS器件,实现其电致发光,并探索了提高电致发光强度的途径,我们得出以下结论:
第一,通过电子束蒸发法,能够制备得到致密的铕掺杂富硅氧化硅薄膜。通过控制铕掺杂富硅氧化硅薄膜沉积过程中的衬底温度,我们发现随着薄膜沉积时衬底温度的升高,原生薄膜的PL逐渐减弱,而热处理后薄膜的PL强度逐渐增强。
第二,发现了在薄膜的沉积过程中,Eu的价态发生了Eu~(3+)-Eu~(2+)的转变。Eu在蒸发源中以Eu~(3+)存在,在沉积的原生薄膜中大部分为Eu~(2+)。这是由于沉积到衬底上的SiO通过夺取Eu_2O_3中的O原子,转变成SiO_2,同时Eu自身被还原为Eu~(2+)。
第三,当热处理温度低于800℃时,铕掺杂富硅氧化硅薄膜PL积分强度随热处理温度的升高而逐渐降低,而当热处理温度高于800℃时,PL积分强度随热处理温度的升高而逐渐增强。样品在1100℃的积分强度几乎为未经热处理样品的11倍,为800℃时的72倍。这种荧光增强是由于薄膜在热处理过程中微结构的变化引起的,并且同时伴随荧光机制的转变。将热处理温度固定为PL强度最强的1100℃,研究了PL强度随热处理时间的变化关系,在时间低于90 min时,PL强度随热处理时间的延长而逐渐增强,当时间再延长时,PL积分强度基本不变。而随后通过荧光寿命测试,我们发现随着热处理温度的升高,荧光寿命在800℃处呈现了一个明显的由ns到us级别的转变过程。分别对应于氧化硅基体缺陷态的发光和Eu~(2+)的4f~65d-4f~7(~8S_(7/2))能级跃迁,并且进一步设计实验验证了高于800℃后的强宽带发光来自于Eu~(2+),随后我们通过TEM,SAED,XRD对薄膜的微观结构进行了表征,发现了随着薄膜热处理温度的升高,EuSiO_3多晶的团簇在薄膜中形成,结晶度不断提高。因此我们认为热处理过程中荧光机制的转变是由薄膜的微结构变化引起。
第四,我们还将铕掺杂富硅氧化硅薄膜制作成ITO/EuSiO/P-Si/Al MOS器件结构,成功实现了薄膜的电致发光。但是器件注入电流相对较大,我们认为是常规热处理形成的较大EuSiO_3颗粒,注入的电子通过颗粒间进行传导,当遇到缺陷复合中心时,电子空穴对发生辐射复合,而发射可见光。我们针对此结构进行了改进,采用p/p~+衬底取代p型衬底,以使得衬底和电极间形成欧姆接触;采用RTP取代常规热处理,以形成更小更均匀的颗粒团簇;通过在铕硅氧薄膜上添加SiO_2层,实现了增大电场,降低注入电流的目的。相较没有添加SiO_2的电致发光器件,在更低的注入电流和偏压下能够实现Eu~(2+)的4f~65d-4f~7能级跃迁而发出的更强电致发光。
Light emitter is one of most important issues silicon-based photonics now facing. Because of the indirect band gap of silicon, making it be not suitable for optical active devices. However, rare-earth (RE) ions have attracted great interest all over the world for its high luminescence intensity, monochromatic and stable performance at room temperature. Therefore, RE-doped silicon based light emitting materials and devices may be the choice of light source of silicon photonics. In this work, photoluminescence (PL) and electroluminescence (EL) performance of Europium (Eu)-doped silicon rich oxide (SRO) thin films have been investigated, to expore its ways as the light emitterof silicon photonics.
Eu-doped SRO films have been prepared by electron beam evaporation (EBE). The dose of Eu was controlled by controlling the dose in the evaporation source. The influence of sample preparation and followed heat treatment on the PL performance is studied in detail. While the main results are summarized as follow:
1) Dense and uniform Eu-doped SRO films can be prepared by the method of EBE. We found PL intensity was dependent on temperature of substrate during deposition process. On the other hand, the PL of as-deposited sample can be increased by post-annealing.
2) A reduction process of Eu~(3+) has been taken place during the film deposition. Eu~(3+) in the evaporation source was reduced to Eu~(2+) in the film during deposition, while SiO get O from Eu_2O_3 to form SiO_2.
3) The luminescence and structure evolution of Eu-doped SRO films were investigated after post-annealing. PL shows significant intensity enhancement after 1100℃annealing. This enhancement is associated with the formation of europium silicate (EuSiO_3), which is confirmed by x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD) and transmission electron microscopy (TEM) results. During annealing, the luminescence mechanism transfers from light emitting of defect related state in SRO film to an energy level transition between 4f~65d and 4f~7(~8S_(7/2)) of Eu~(3+).
4) Eu-doped SRO films have been used to produce the ITO/Eu_xSi_yO_z/p-Si/AI MOS device structures to realize its EL. The MOS devices emitted visible light originated from radiative recombination of defect related state in SRO film. However, the EuSiO_3 particles formed during high temperature annealing provided a channel for carries and resulted in a large injection current. After improving the device structure, more intense EL from the 4f~65d-4f~7 energy levels of Eu~(2+) was emitted from device with a lower injected current.
铕掺杂的富硅氧化硅薄膜是通过电子束蒸发法(EBE)进行制备,铕的掺杂剂量是通过蒸发源中的掺杂剂量进行控制。通过对薄膜制备条件以及后续热处理过程与发光特性(PL)间的关系进行了详细研究,并将薄膜制备成MOS器件,实现其电致发光,并探索了提高电致发光强度的途径,我们得出以下结论:
第一,通过电子束蒸发法,能够制备得到致密的铕掺杂富硅氧化硅薄膜。通过控制铕掺杂富硅氧化硅薄膜沉积过程中的衬底温度,我们发现随着薄膜沉积时衬底温度的升高,原生薄膜的PL逐渐减弱,而热处理后薄膜的PL强度逐渐增强。
第二,发现了在薄膜的沉积过程中,Eu的价态发生了Eu~(3+)-Eu~(2+)的转变。Eu在蒸发源中以Eu~(3+)存在,在沉积的原生薄膜中大部分为Eu~(2+)。这是由于沉积到衬底上的SiO通过夺取Eu_2O_3中的O原子,转变成SiO_2,同时Eu自身被还原为Eu~(2+)。
第三,当热处理温度低于800℃时,铕掺杂富硅氧化硅薄膜PL积分强度随热处理温度的升高而逐渐降低,而当热处理温度高于800℃时,PL积分强度随热处理温度的升高而逐渐增强。样品在1100℃的积分强度几乎为未经热处理样品的11倍,为800℃时的72倍。这种荧光增强是由于薄膜在热处理过程中微结构的变化引起的,并且同时伴随荧光机制的转变。将热处理温度固定为PL强度最强的1100℃,研究了PL强度随热处理时间的变化关系,在时间低于90 min时,PL强度随热处理时间的延长而逐渐增强,当时间再延长时,PL积分强度基本不变。而随后通过荧光寿命测试,我们发现随着热处理温度的升高,荧光寿命在800℃处呈现了一个明显的由ns到us级别的转变过程。分别对应于氧化硅基体缺陷态的发光和Eu~(2+)的4f~65d-4f~7(~8S_(7/2))能级跃迁,并且进一步设计实验验证了高于800℃后的强宽带发光来自于Eu~(2+),随后我们通过TEM,SAED,XRD对薄膜的微观结构进行了表征,发现了随着薄膜热处理温度的升高,EuSiO_3多晶的团簇在薄膜中形成,结晶度不断提高。因此我们认为热处理过程中荧光机制的转变是由薄膜的微结构变化引起。
第四,我们还将铕掺杂富硅氧化硅薄膜制作成ITO/EuSiO/P-Si/Al MOS器件结构,成功实现了薄膜的电致发光。但是器件注入电流相对较大,我们认为是常规热处理形成的较大EuSiO_3颗粒,注入的电子通过颗粒间进行传导,当遇到缺陷复合中心时,电子空穴对发生辐射复合,而发射可见光。我们针对此结构进行了改进,采用p/p~+衬底取代p型衬底,以使得衬底和电极间形成欧姆接触;采用RTP取代常规热处理,以形成更小更均匀的颗粒团簇;通过在铕硅氧薄膜上添加SiO_2层,实现了增大电场,降低注入电流的目的。相较没有添加SiO_2的电致发光器件,在更低的注入电流和偏压下能够实现Eu~(2+)的4f~65d-4f~7能级跃迁而发出的更强电致发光。
Light emitter is one of most important issues silicon-based photonics now facing. Because of the indirect band gap of silicon, making it be not suitable for optical active devices. However, rare-earth (RE) ions have attracted great interest all over the world for its high luminescence intensity, monochromatic and stable performance at room temperature. Therefore, RE-doped silicon based light emitting materials and devices may be the choice of light source of silicon photonics. In this work, photoluminescence (PL) and electroluminescence (EL) performance of Europium (Eu)-doped silicon rich oxide (SRO) thin films have been investigated, to expore its ways as the light emitterof silicon photonics.
Eu-doped SRO films have been prepared by electron beam evaporation (EBE). The dose of Eu was controlled by controlling the dose in the evaporation source. The influence of sample preparation and followed heat treatment on the PL performance is studied in detail. While the main results are summarized as follow:
1) Dense and uniform Eu-doped SRO films can be prepared by the method of EBE. We found PL intensity was dependent on temperature of substrate during deposition process. On the other hand, the PL of as-deposited sample can be increased by post-annealing.
2) A reduction process of Eu~(3+) has been taken place during the film deposition. Eu~(3+) in the evaporation source was reduced to Eu~(2+) in the film during deposition, while SiO get O from Eu_2O_3 to form SiO_2.
3) The luminescence and structure evolution of Eu-doped SRO films were investigated after post-annealing. PL shows significant intensity enhancement after 1100℃annealing. This enhancement is associated with the formation of europium silicate (EuSiO_3), which is confirmed by x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD) and transmission electron microscopy (TEM) results. During annealing, the luminescence mechanism transfers from light emitting of defect related state in SRO film to an energy level transition between 4f~65d and 4f~7(~8S_(7/2)) of Eu~(3+).
4) Eu-doped SRO films have been used to produce the ITO/Eu_xSi_yO_z/p-Si/AI MOS device structures to realize its EL. The MOS devices emitted visible light originated from radiative recombination of defect related state in SRO film. However, the EuSiO_3 particles formed during high temperature annealing provided a channel for carries and resulted in a large injection current. After improving the device structure, more intense EL from the 4f~65d-4f~7 energy levels of Eu~(2+) was emitted from device with a lower injected current.
引文
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