ZnO薄膜制备及其光、电性能研究
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摘要
六方纤锌矿结构的ZnO材料由于其具有独特的电学和光学性能,在压电、气体传感器、光电器件等领域有广泛的应用。本文采用Sol-gel法和RF磁控溅射法在玻璃和Si(111)衬底上沉积了ZnO薄膜,并对薄膜的结构、表面形貌、电学性能和光学性能等进行了表征。
以二水合醋酸锌、乙二醇甲醚、乙醇胺、二水合氯化镁等为前驱物,在载玻片衬底上Sol-gel法制备了ZnO薄膜,系统研究了掺杂量、溶液浓度、热处理温度等对薄膜性能的影响。实验结果表明,适量Li或Mg的掺杂可促进薄膜(002)定向生长,并明显提高材料的电阻率;溶液浓度为0.45mol/L、旋涂7次、在610℃下热处理的Li/Mg共掺(Li/Zn = 0.10, Mg/Zn = 0.04)ZnO薄膜呈现极好的(002)定向性,定向指数达0.961,电阻率达6.0×107?cm。薄膜从光致发光研究表明, Li掺杂ZnO薄膜在PL谱上出现了403nm的发光峰,同时ZnO的带边发射(NBE)峰(371nm)消失,而Mg掺杂后不改变NBE峰的位置。随Li和/或Mg掺杂浓度的升高,ZnO薄膜材料的深能级发光峰(DLE)变弱。
首次采用高RF磁控溅射功率(550W)制备了(100)择优取向的ZnO,其定向指数可达0.752,而在较低的功率(200～380W)下溅射,薄膜呈现很好的(101)取向,定向指数达0.799;基片加热至250℃、溅射功率200W时,制备的ZnO薄膜则表现为(002)择优取向性,定向指数为0.742。从原子堆积方式的角度提出了不同择优取向薄膜的生长机理。对三种择优取向薄膜的晶格常数的测试结果表明,(002)取向的晶胞较小,而(101)取向的薄膜晶胞最大。(100)取向薄膜的PL谱以Li的杂质能级峰(399nm)为主,(002)取向的薄膜以Zni缺陷的能级峰(420nm)为主,而(101)取向薄膜主要为带边发射(384nm);薄膜的电阻率随溅射功率的增加而增大;薄膜的表面形貌表明,(100)取向的薄膜与其它取向薄膜相比晶粒更加细密。作为对比,实验还在Si(111)衬底上磁控溅射了ZnO薄膜,结果表明,RF功率在200～550W范围内均可获得(002)定向性极好薄膜,而在100W功率下,薄膜呈现(101)择优取向。
ZnO material with hexagonal wurtzite structure has been widely used in piezoelectric, optoelectronic devices and sensors due to its unique electrical and optical properties. In this paper, two methods, sol-gel and RF magnetron sputtering, were employed to fabricate ZnO thin films. The structural, electrical and optical characteristics of ZnO films were investigated using XRD, AFM, SEM, EDS and photoluminescent (PL) measurements.
Li+, Mg2+ and Li+/Mg2+ doped ZnO films were prepared on lime-glass substrate by sol-gel method using zinc acetate, 2-methoxyethanol and monoethanolamine as starting materials, and the effects of processing parameters such as dopants, solution concentration, postheating temperature and the film thickness on the properties of ZnO films were discussed. The results showed that proper amount of Li+ or Mg2+ dopants could obviously improve the cystallization and the preferential C-orientation, as well as the resistivity of ZnO films. For the Li/Mg co-doped ZnO film (Li/Zn=0.10, Mg/Zn=0.04) annealed at 610℃, the oriented degree of (002) plane(OD002) and the resistivity reached 0.961 and 6.0×107?cm, respectively. The photoluminescent results showed that the 403nm PL peak was induced by Li acceptor level (about 0.29eV), and for the Li-doped ZnO films the NBE peak near 371nm disappeared. The intensities of DLE peaks near 452nm and 470nm decrease with the increase of Li or Mg dopants.
The ZnO (100) thin film with OD100 of 0.752 was successfully deposited on lime-glass substrate under extremely high RF power (550W) by magnetron sputtering, while deposited under low RF power (100~380W), the film preferentially oriented along (101) with OD101 of 0.799. However, when the substrate heated to 250℃, the films deposited at 200W preferably grew along (002) with the OD002 of 0.742. The XRD results indicated that the cell parameters of ZnO film with C-orientation was smaller than that with (100) and (101) orientation, which was probably due to the different amount of defects in the three kinds of films. The PL spectra also proved that
以二水合醋酸锌、乙二醇甲醚、乙醇胺、二水合氯化镁等为前驱物,在载玻片衬底上Sol-gel法制备了ZnO薄膜,系统研究了掺杂量、溶液浓度、热处理温度等对薄膜性能的影响。实验结果表明,适量Li或Mg的掺杂可促进薄膜(002)定向生长,并明显提高材料的电阻率;溶液浓度为0.45mol/L、旋涂7次、在610℃下热处理的Li/Mg共掺(Li/Zn = 0.10, Mg/Zn = 0.04)ZnO薄膜呈现极好的(002)定向性,定向指数达0.961,电阻率达6.0×107?cm。薄膜从光致发光研究表明, Li掺杂ZnO薄膜在PL谱上出现了403nm的发光峰,同时ZnO的带边发射(NBE)峰(371nm)消失,而Mg掺杂后不改变NBE峰的位置。随Li和/或Mg掺杂浓度的升高,ZnO薄膜材料的深能级发光峰(DLE)变弱。
首次采用高RF磁控溅射功率(550W)制备了(100)择优取向的ZnO,其定向指数可达0.752,而在较低的功率(200～380W)下溅射,薄膜呈现很好的(101)取向,定向指数达0.799;基片加热至250℃、溅射功率200W时,制备的ZnO薄膜则表现为(002)择优取向性,定向指数为0.742。从原子堆积方式的角度提出了不同择优取向薄膜的生长机理。对三种择优取向薄膜的晶格常数的测试结果表明,(002)取向的晶胞较小,而(101)取向的薄膜晶胞最大。(100)取向薄膜的PL谱以Li的杂质能级峰(399nm)为主,(002)取向的薄膜以Zni缺陷的能级峰(420nm)为主,而(101)取向薄膜主要为带边发射(384nm);薄膜的电阻率随溅射功率的增加而增大;薄膜的表面形貌表明,(100)取向的薄膜与其它取向薄膜相比晶粒更加细密。作为对比,实验还在Si(111)衬底上磁控溅射了ZnO薄膜,结果表明,RF功率在200～550W范围内均可获得(002)定向性极好薄膜,而在100W功率下,薄膜呈现(101)择优取向。
ZnO material with hexagonal wurtzite structure has been widely used in piezoelectric, optoelectronic devices and sensors due to its unique electrical and optical properties. In this paper, two methods, sol-gel and RF magnetron sputtering, were employed to fabricate ZnO thin films. The structural, electrical and optical characteristics of ZnO films were investigated using XRD, AFM, SEM, EDS and photoluminescent (PL) measurements.
Li+, Mg2+ and Li+/Mg2+ doped ZnO films were prepared on lime-glass substrate by sol-gel method using zinc acetate, 2-methoxyethanol and monoethanolamine as starting materials, and the effects of processing parameters such as dopants, solution concentration, postheating temperature and the film thickness on the properties of ZnO films were discussed. The results showed that proper amount of Li+ or Mg2+ dopants could obviously improve the cystallization and the preferential C-orientation, as well as the resistivity of ZnO films. For the Li/Mg co-doped ZnO film (Li/Zn=0.10, Mg/Zn=0.04) annealed at 610℃, the oriented degree of (002) plane(OD002) and the resistivity reached 0.961 and 6.0×107?cm, respectively. The photoluminescent results showed that the 403nm PL peak was induced by Li acceptor level (about 0.29eV), and for the Li-doped ZnO films the NBE peak near 371nm disappeared. The intensities of DLE peaks near 452nm and 470nm decrease with the increase of Li or Mg dopants.
The ZnO (100) thin film with OD100 of 0.752 was successfully deposited on lime-glass substrate under extremely high RF power (550W) by magnetron sputtering, while deposited under low RF power (100~380W), the film preferentially oriented along (101) with OD101 of 0.799. However, when the substrate heated to 250℃, the films deposited at 200W preferably grew along (002) with the OD002 of 0.742. The XRD results indicated that the cell parameters of ZnO film with C-orientation was smaller than that with (100) and (101) orientation, which was probably due to the different amount of defects in the three kinds of films. The PL spectra also proved that
引文
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