掺铝氧化锌薄膜的相关特性研究
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摘要
近年来,由于Al掺杂ZnO薄膜具有与ITO薄膜相比拟的光电性能,又因其原料丰富、价格低廉以及在氢等离子体环境下稳定等优点,已经成为透明导电薄膜领域的研究和应用热点之一。将表面织构后的ZnO:Al(AZO)薄膜代替SnO_2薄膜作为微晶硅薄膜太阳能电池的前电极得到越来越广泛的关注。
为此本文分别利用直流脉冲反应磁控溅射(DCP-sputtering)和直流磁控反应溅射(DC-sputtering)技术在玻璃衬底上制备了AZO透明导电薄膜。利用扫描电子显微镜(SEM)、X射线衍射(XRD)、四探针和分光光度计分别研究了沉积参数对AZO薄膜的结构、电学和光学特性的影响。利用“包络法”和椭圆光谱法分别拟合了DCP-sputtering和DC-sputtering制备的AZO薄膜的光学常数。最后采用5%的氯化铵(NH_4Cl)溶液对制备的AZO薄膜进行表面织构,深入研究了表面织构过程和织构机制。此外还对比研究了DCP-sputtering和DC-sputtering技术对AZO薄膜的表面织构的影响。研究结果表明:
(1) DCP-sputtering制备的AZO薄膜丧失了c轴(002)择优取向,该结果可能归结于晶面能的演变和生长模式的转变。随着衬底温度由210℃升高到290℃,AZO薄膜的电阻率先减小后略有升高,分别从衬底温度、薄膜生长机制、薄膜晶体结构和薄膜表面结构的角度解释了电阻率的变化趋势。随着衬底温度的升高,AZO薄膜的吸收边先发生了蓝移,高于270℃后,又发生了红移。利用Burstein-Moss效应分析了AZO薄膜吸收边的蓝移和红移。
(2) DC-sputtering制备的AZO薄膜均出现了ZnO-(002)和(103)两个衍射峰,并在衬底温度为200℃时,AZO样品表现出明显的c轴择优取向,说明薄膜的结晶状态在衬底温度为200℃附近最好。电阻率在衬底温度为200℃时取得最小值2.93×10~(-3)Ω·cm。
(3)“包络法”拟合的DCP-sputtering制备的AZO薄膜的折射率在可见光范围内基本上为一恒值(n≈2)。椭圆光谱法拟合的DC-sputtering技术制备的AZO薄膜的介电常数的实部和虚部在可见光范围内基本上保持不变,其值分别为3.4和0.25,且在光吸收边附近均出现突变。相应地,随着衬底温度由170℃增加到210℃,吸收边出现了蓝移和红移的现象。(4)NH_4Cl溶液容易控制DCP-sputtering制备的AZO薄膜的表面织构过程,并且可以获得有效的绒面。表面织构后,薄膜在可见光波段的平均反射率急剧的从12%降低到7.86%,且电阻率略有增大。而对于DC-sputtering制备的AZO薄膜却没有获得明显的织构表面。从应力和致密度的角度对实验结果作了合理解释。
In recent years,Al-doped zinc oxide(AZO) films has been a hot topic in transparent conductive film field not only because of their comparable optical and electrical properties to ITO films,but also because of their low cost,abundance in natural resource,and high stability in a hydrogen plasma environment.Surface textured AZO film,an alternative front contact material of SnO_2 in microcrystalline silicon film solar cells,has been paid much attention to.
In this paper,AZO films were prepared on glass substrate by direct current pulse reactive magnetron sputtering(DCP-sputtering) and direct current reactive magnetron sputtering(DC-sputtering),respectively.The effect of deposition parameters on the structural,electrical,and optical properties of AZO films was investigated systematically by scanning electron microscopy(SEM),x-ray diffractometry(XRD), four point probe and UV-VIS-IR spectrophotometry,respectively.The optical constants of the as-deposited AZO films were fitted by envelop method(EM) and spectroscopic ellipsometry(SE),respectively.In addition,the as-deposited AZO films were textured by 5%NH_4Cl aqueous solution.And the texture process and texture mechanism were deeply investigated.The effect of DCP-sputtering and DC-sputtering was also comparably studied on the surface texture of the as-deposited AZO films by using NH_4Cl aqueous solution.The results indicate:
(1) The as-deposited AZO films by DCP-sputtering technique lost a(002) c-axis preferential orientation,which might originate from the evolution of the crystal face energy and the transition of film grow mode.The resistivity decreased firstly and then slightly increased at substrate temperature increasing from 210℃to 290℃.The change tendency of the resistivity was explained from the viewpoint of substrate temperature,film grow mechanism,crystal structure,and film surface structure, respectively.The blue and red shifts of the optical absorption edge occurred at substrate temperature below and above 270℃,respectively.The blue and red shifts were explained by Burstein-Moss effect.
(2) The as-deposited AZO films by DC-sputtering technique exhibited ZnO-(002) and (103) characteristic diffraction peaks.In particular,the AZO film deposited at a substrate temperature of 200℃exhibited a strongest(002) preferential orientation. The resistivity decreased to 2.93×10~(-3)Ω·cm when substrate temperature increased from 170℃to 200℃and then increased at substrate temperature over 200℃.
(3) The average refractive of AZO films prepared by DCP-sputtering at different substrate temperatures nearly keep constant(n≈2) in the visible wavelength range.SE was used to determine the dielectric constants of AZO films prepared by DCsputtering technique at different substrate temperatures.The real and imaginary parts of dielectric constants of AZO films demonstrate a slight change in the visible light range,while show a sharp change near the optical absorption edge.And the average values ofε_1 andε_2 in the visible light range are 3.4 and 0.25,respectively.The shift of the absorption edge was observed correspondly with the substrate temperature increasing from 170℃to 210℃.
(4) The NH_4Cl aqueous solution was able to easily control the surface texture of the as-deposited AZO films by DCP-spttering and obtain an effective surface texture.The reflectivity of the textured AZO films in the visible region drastically decreased from 12%to 7.86%and the resistivity slightly increased.While the as-deposited AZO films by DC-sputtering showed no apparent surface texture.The result was able to be accounted for by relative stress and film compactability.
为此本文分别利用直流脉冲反应磁控溅射(DCP-sputtering)和直流磁控反应溅射(DC-sputtering)技术在玻璃衬底上制备了AZO透明导电薄膜。利用扫描电子显微镜(SEM)、X射线衍射(XRD)、四探针和分光光度计分别研究了沉积参数对AZO薄膜的结构、电学和光学特性的影响。利用“包络法”和椭圆光谱法分别拟合了DCP-sputtering和DC-sputtering制备的AZO薄膜的光学常数。最后采用5%的氯化铵(NH_4Cl)溶液对制备的AZO薄膜进行表面织构,深入研究了表面织构过程和织构机制。此外还对比研究了DCP-sputtering和DC-sputtering技术对AZO薄膜的表面织构的影响。研究结果表明:
(1) DCP-sputtering制备的AZO薄膜丧失了c轴(002)择优取向,该结果可能归结于晶面能的演变和生长模式的转变。随着衬底温度由210℃升高到290℃,AZO薄膜的电阻率先减小后略有升高,分别从衬底温度、薄膜生长机制、薄膜晶体结构和薄膜表面结构的角度解释了电阻率的变化趋势。随着衬底温度的升高,AZO薄膜的吸收边先发生了蓝移,高于270℃后,又发生了红移。利用Burstein-Moss效应分析了AZO薄膜吸收边的蓝移和红移。
(2) DC-sputtering制备的AZO薄膜均出现了ZnO-(002)和(103)两个衍射峰,并在衬底温度为200℃时,AZO样品表现出明显的c轴择优取向,说明薄膜的结晶状态在衬底温度为200℃附近最好。电阻率在衬底温度为200℃时取得最小值2.93×10~(-3)Ω·cm。
(3)“包络法”拟合的DCP-sputtering制备的AZO薄膜的折射率在可见光范围内基本上为一恒值(n≈2)。椭圆光谱法拟合的DC-sputtering技术制备的AZO薄膜的介电常数的实部和虚部在可见光范围内基本上保持不变,其值分别为3.4和0.25,且在光吸收边附近均出现突变。相应地,随着衬底温度由170℃增加到210℃,吸收边出现了蓝移和红移的现象。(4)NH_4Cl溶液容易控制DCP-sputtering制备的AZO薄膜的表面织构过程,并且可以获得有效的绒面。表面织构后,薄膜在可见光波段的平均反射率急剧的从12%降低到7.86%,且电阻率略有增大。而对于DC-sputtering制备的AZO薄膜却没有获得明显的织构表面。从应力和致密度的角度对实验结果作了合理解释。
In recent years,Al-doped zinc oxide(AZO) films has been a hot topic in transparent conductive film field not only because of their comparable optical and electrical properties to ITO films,but also because of their low cost,abundance in natural resource,and high stability in a hydrogen plasma environment.Surface textured AZO film,an alternative front contact material of SnO_2 in microcrystalline silicon film solar cells,has been paid much attention to.
In this paper,AZO films were prepared on glass substrate by direct current pulse reactive magnetron sputtering(DCP-sputtering) and direct current reactive magnetron sputtering(DC-sputtering),respectively.The effect of deposition parameters on the structural,electrical,and optical properties of AZO films was investigated systematically by scanning electron microscopy(SEM),x-ray diffractometry(XRD), four point probe and UV-VIS-IR spectrophotometry,respectively.The optical constants of the as-deposited AZO films were fitted by envelop method(EM) and spectroscopic ellipsometry(SE),respectively.In addition,the as-deposited AZO films were textured by 5%NH_4Cl aqueous solution.And the texture process and texture mechanism were deeply investigated.The effect of DCP-sputtering and DC-sputtering was also comparably studied on the surface texture of the as-deposited AZO films by using NH_4Cl aqueous solution.The results indicate:
(1) The as-deposited AZO films by DCP-sputtering technique lost a(002) c-axis preferential orientation,which might originate from the evolution of the crystal face energy and the transition of film grow mode.The resistivity decreased firstly and then slightly increased at substrate temperature increasing from 210℃to 290℃.The change tendency of the resistivity was explained from the viewpoint of substrate temperature,film grow mechanism,crystal structure,and film surface structure, respectively.The blue and red shifts of the optical absorption edge occurred at substrate temperature below and above 270℃,respectively.The blue and red shifts were explained by Burstein-Moss effect.
(2) The as-deposited AZO films by DC-sputtering technique exhibited ZnO-(002) and (103) characteristic diffraction peaks.In particular,the AZO film deposited at a substrate temperature of 200℃exhibited a strongest(002) preferential orientation. The resistivity decreased to 2.93×10~(-3)Ω·cm when substrate temperature increased from 170℃to 200℃and then increased at substrate temperature over 200℃.
(3) The average refractive of AZO films prepared by DCP-sputtering at different substrate temperatures nearly keep constant(n≈2) in the visible wavelength range.SE was used to determine the dielectric constants of AZO films prepared by DCsputtering technique at different substrate temperatures.The real and imaginary parts of dielectric constants of AZO films demonstrate a slight change in the visible light range,while show a sharp change near the optical absorption edge.And the average values ofε_1 andε_2 in the visible light range are 3.4 and 0.25,respectively.The shift of the absorption edge was observed correspondly with the substrate temperature increasing from 170℃to 210℃.
(4) The NH_4Cl aqueous solution was able to easily control the surface texture of the as-deposited AZO films by DCP-spttering and obtain an effective surface texture.The reflectivity of the textured AZO films in the visible region drastically decreased from 12%to 7.86%and the resistivity slightly increased.While the as-deposited AZO films by DC-sputtering showed no apparent surface texture.The result was able to be accounted for by relative stress and film compactability.
引文
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