[100]取向Al-Ti共掺杂ZnO薄膜的制备与光电性能研究

采用常压固相烧结法制备了Al-Ti共掺ZnO靶材, 采用射频磁控溅射技术及真空退火工艺, 在普通玻璃衬底上制备了具有[100]取向Al-Ti共掺杂ZnO薄膜(ZATO). 采用X射线衍射(XRD)、扫描电子显微镜(SEM)对ZATO薄膜的生长机理、显微结构、形貌进行了测试分析, 用四探针测试仪、紫外-可见分光光度计及荧光光谱仪对ZATO薄膜的光电性能进行了测试分析. 结果表明, ZATO薄膜经500℃保温3h退火后, 择优取向由(002)向(100)方向转变; 此时, 衍射谱上还观察到超点阵衍射线条. [100]取向ZATO薄膜的光学带隙从退火前的3.29降至2.86, 平均可见光透过率从90%降至70%, 表现为一般的透过性; 而电阻率则从1.89×10^-2Ω·cm降至1.25×10^-3Ω·cm, 呈现较好的导电性. 薄膜中均出现了380nm附近的带边发射(NBE)峰以及410、564nm的深能级发射峰, 且经500℃保温3h退火后, 这些峰的位置并未改变, 但峰强均明显减弱. 对上述实验机理进行了分析讨论.     

沉积气压对磁控溅射制备ZnO薄膜的结构与光学性能影响

采用CS-400型射频磁控溅射仪在Si(111)和石英基底上成功的制备了ZnO薄膜,分别用XRD、SEM、紫外-可见光分光光度计和荧光分光光度计表征样品的结构和光学性质.实验表明,采用射频磁控溅射制备的ZnO薄膜具有六角纤锌矿结构的(002)峰和(101)峰的两种取向.在沉积气压>1.0Pa时所制备的ZnO薄膜具有(002)择优取向,并且十分稳定.SEM图表明,ZnO薄膜颗粒大小较为均匀,晶粒尺寸随着气压升高而变小,沉积气压不同时,薄膜样品的生长方式有所差异.在400～1000nm范围内,可以看出除O.5Pa下制备的ZnO薄膜外,其余ZnO薄膜在可见光区域的平均透过率超过80%,吸收边在380nm附近,所对应的光学带隙约为3.23～3.27eV,并随着沉积气压上升而变大.ZnO薄膜的PL谱上观察到了392nm的近紫外峰和419nm的蓝峰;沉积气压对Zno薄膜的发光峰位和峰强有影响.     

稀土Nd掺杂纳米SnO2薄膜特性

对采用真空气相沉积法在玻璃衬底上制备的稀土Nd掺杂的SnO2薄膜,进行结构、电学及光学特性的测试分析.实验表明:氧化、热处理条件为500 ℃、45 min时样品性能好.采用一步成膜工艺法制备的SnO2薄膜晶粒度较小,随掺Nd浓度的增大,从31.516 nm减小到25.927 nm;两步成膜工艺法制备的SnO2薄膜晶粒度随掺Nd浓度的增大,从45.692 nm增至66.256 nm.XRD分析,掺Nd(5 at%)薄膜沿[110]、[101]晶向的衍射峰加强,薄膜呈多晶结构.掺Nd可使薄膜透光率下降,而薄膜的薄层电阻随热处理温度升高和掺Nd浓度的增大,呈先降后升趋势.     

2-(2-羟基苯基)苯并咪唑锌的合成及其光谱性能研究

合成了一种纯蓝的发光材料2-(2-羟基苯基)苯并咪唑锌(Zn(pbm)2),用元素分析、核磁共振、红外光谱、紫外-可见光吸收光谱、循环伏安曲线、原子力显微镜以及光致发光光谱、热重等表征了材料的结构、光学带隙、能带结构、成膜性能、发光性能以及热稳定性.实验结果表明,配合物具有较好的热稳定性;在DMSO溶液中Zn(pbm)2的紫外吸收峰波长为299、334、357nm;光学带隙为3.03eV.利用真空热蒸镀法可以得到均匀致密的Zn(pbm)2薄膜,其粗糙度为7.05nm.在365nm紫外光的激发下,产生发光峰在445nm附近,半高宽(FWHM)为81nm的纯蓝光发射.     

水热处理对ZnO薄膜微结构及光学性能的影响

基于溶液工艺和水热处理制备了ZnO薄膜。采用椭圆偏振光谱分析仪,原子力显微镜,X射线衍射仪研究和分析了水热处理温度对薄膜的微观形貌,光学特性,晶体结构的影响。实验结果表明,水热处理温度由110℃升高到130℃,薄膜光学带隙由3.19eV增大到3.31eV,而薄膜表面粗糙度从19.3nm降到12.9nm。然而,当处理温度超过140℃后,与130℃下处理的膜相比质量显著劣化。此外,130℃下水热处理的膜与500℃下高温退火的膜对比表明水热法有相似的光学特性,同时,XRD分析表明水热处理能改善晶体特性。证明了利用水热处理能够极大地降低溶液法制备ZnO薄膜所需的退火温度。     

后退火对射频磁控溅射制备β-Ga_2O_3薄膜的影响

采用射频磁控溅射法制备了氧化镓(Ga_2O_3)薄膜,计算了薄膜的O/Ga摩尔比,比值为1.57。研究了后退火对薄膜结构,形貌特征和光学带隙的影响。X射线衍射(XRD)结果表明,退火前的Ga_2O_3薄膜是一种无定形结构。在600℃氧气氛中退火2h后,薄膜开始出现β-Ga_2O_3的(■01)衍射峰;随着退火温度的升高,β-Ga_2O_3(■01)衍射峰进一步增强,并且半高宽从0.61°减小到0.49°。原子力显微镜(AFM)测试结果表明,退火前后薄膜表面的均方根粗糙度从3.47 nm增加到了7.08 nm,晶粒尺寸从19 nm增加到了53 nm。紫外-可见分光光度计(UV-VIS)测试结果表明Ga_2O_3薄膜在250 nm-1500 nm波长范围内的平均透过率在85%以上。利用Tauc公式计算了Ga_2O_3薄膜的光学带隙,带隙宽度在(4.85-5.06)eV之间,且随退火温度增加而减小。分析了表面形貌、光学带隙与薄膜结构之间的关系。     

衬底温度对Mg0.1Zn0.9O薄膜结构及光学性能的影响

利用射频磁控溅射技术在不同温度的(100)Si和玻璃衬底上成功地制备了c轴择优取向的Mg0.1Zn0.9O薄膜.通过X射线衍射(XRD)、场发射扫描电镜(FESEM)、紫外可见光分光光度计和光致发光谱研究了衬底温度对Mg0.1Zn0.9O薄膜结构、表面形貌和光学性能的影响,结果表明,在衬底温度为400℃时生长的Mg0.1Zn0.9O薄膜具有很好的c轴取向和较好的光学性能.用激发波长为300nm的氙灯作为激发光源得到不同衬底温度下Mg0.1Zn0.9O薄膜的室温PL谱.分析表明,紫外发光峰与薄膜的结晶质量密切相关,蓝光发射与氧空位有关.简单探讨了衬底温度影响紫外光致发光峰红移和蓝移的可能机理.     

Zn掺杂Sn2S3薄膜的特性

高纯Sn和S粉按1∶0.41%(质量分数)配比,均匀掺入9%(质量分数)的高纯Zn粉,单源共蒸发沉积薄膜后再进行热处理,得到Sn2S3∶Zn薄膜。XRD分析显示,380℃,55min热处理得到简单正交晶系的纯Sn2S3薄膜。掺Zn 9%(质量分数)的薄膜经370℃热处理15min得到的薄膜仍属简单正交晶系。掺Zn后Sn2S3薄膜的表面均匀和致密性变好,平均晶粒尺寸从未掺Zn时的35.69nm增加到58.80nm。Sn2S3薄膜的导电类型均为N型,掺Zn后薄膜的电阻率为60.5(Ω·cm),比未掺杂时降低1个数量级。Sn2S3薄膜的直接光学带隙为1.85eV,本征吸收边为551nm;Sn2S3∶Zn 9%(质量分数)薄膜的光学带隙1.41eV,本征吸收边873nm发生红移,Sn2S3薄膜的光吸收系数均达到105cm-1。     

热丝辅助MW ECR CVD法高速沉积优质氢化非晶硅薄膜

我们用热丝辅助MW ECRCVD系统,在热丝温度分别为0、1350、1400、1450、1500、1600和1700℃时制备出a-SiH薄膜.通过膜厚测定,红外光谱分析光、暗电导测量等手段,分析了其沉积速率、光敏性及光学带隙的变化规律.结果表明沉积速率和薄膜质量均得到明显的提高,沉积速率超过3nm/s,光暗电导之比提高到6×105.找到最佳辅助热丝温度为1450℃.通过对带隙值的分析,发现当带隙值在1.6～1.7范围内时,薄膜几乎都具有105以上的光暗电导之比.     

Sb掺杂Sn_2S_3薄膜的制备及光学特性

真空蒸发制备Sb掺杂Sn2S3多晶薄膜(玻璃衬底),研究不同比例Sb掺杂对Sn2S3薄膜的结构、表面形貌、化学组分及光学特性的影响。实验给出5%掺Sb的薄膜经380℃热处理30min(氮气保护)得到正交晶系的Sn2S3∶Sb多晶薄膜,薄膜表面颗粒大小均匀,膜面致密有轻微颗粒聚集现象。薄膜体内Sn与S化学计量比为1∶1.49,掺Sb后为1∶0.543,薄膜中Sn、S、Sb分别以Sn2+、Sn4+、S2-、Sb5+存在。纯Sn2S3薄膜的光透过率在350~500nm波长范围内基本为零,随着波长增大,光透过率增加,其直接光学带隙为2.2eV,吸收边为564nm;掺Sb后薄膜的光透率明显降低,光学带隙为1.395eV比未掺杂时减小0.805eV,吸收边发生红移为889nm。     

Influence of Fe dopant concentration and annealing temperature on the structural and optical properties of ZnO thin films deposited by sol–gel method

Nanostructured Fe doped ZnO thin films were deposited onto glass substrates by sol–gel spin coating method. Influence of Fe doping concentration and annealing temperature on the structural, compositional, morphological and optical properties were investigated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV–Vis spectroscopy and photoluminescence (PL) measurements. XRD analysis showed that all the films prepared in this work possessed a hexagonal wurtzite structure and were preferentially oriented along the c-axis. Pure ZnO thin films possessed extensive strain, whereas Fe doped films possessed compressive strain. In the doped films, least value of stress and strain was observed in the 0.5 at.% Fe doped thin film, annealed at 873 K. Average crystallite size was not significantly affected by Fe doping, but it increased from 15.57 to 17.79 nm with increase in annealing temperature from 673 to 873 K. Fe ions are present in +3 oxidation state as revealed by XPS analysis of the 0.5 at.% Fe doped film. Surface morphology is greatly affected by changes in Fe doping concentration and annealing temperature which is evident in the SEM images. The increase in optical band gap from 3.21 to 3.25 eV, with increase in dopant concentration was attributed to Moss–Burstein shift. But increase in annealing temperature from 673 to 873 K caused a decrease in band gap from 3.22 to 3.20 eV. PL spectra showed emissions due to excitonic combinations in the UV region and defect related emissions in the visible region in all the investigated films.     

Effects of annealing temperature on the structure and photoluminescence properties of ZnO films

Zinc oxide (ZnO) films with c-orientation were deposited on Si (1 1 1) substrates at room temperature (RT) by RF-magnetron sputtering. Violet (394 and 412 nm) and green (560 and 588 nm) photoluminescence (PL) were observed from the as-deposited and annealed samples. The PL intensity was increasing with increasing annealing temperature (T_a). The 412 nm violet peak shifted from 412 to 407 nm and the 394 nm violet peak shifted from 394 to 399 nm on increasing the temperature from 500 to 900 °C, whereas no shift in PL green peaks was observed over the whole range of temperature examined. The 412 nm violet luminescence is ascribed to radiative defects related to the interface traps existing at grain boundaries. With the increase of T_a, the stress in the films changed from compressive to tensile, which is believed to have resulted in the observed 412 nm violet emission peak shifts from 412-407 nm. The 394 nm violet luminescence observed is attributed to free excitonic emission, and the increase of the crystal size may result in the 394 nm violet emission peak shifts from 394 to 399 nm. The other two PL bands located at 560 and 588 nm are attributed to oxygen deficiency.     

AlSb多晶薄膜材料的性能研究

采用共蒸法制备了新型AlSb多晶薄膜. 通过XRF、XRD、Hall测试及电导率温度关系等研究了AlSb多晶薄膜的组分、结构及性能. 分析表明,刚沉积的AlSb薄膜为非晶相,在540℃以上退火转变为AlSb相,转变的程度取决于退火的温度及Al、Sb的原子配比,其中N_Al∶N_Sb为47.2∶52.8,580℃退火后的薄膜多晶转变最为明显,结晶度较高;测试结果表明,退火后的AlSb薄膜为p型间接带隙半导体,载流子浓度为10¹⁹cm^-1,吸收系数为10⁴,而且在升降温阶段电导率发生不可逆变化. 这种薄膜用于TCO/CdS/AlSb结构的太阳电池器件中已经得到200mV左右的开路电压.     

Enhanced H2 sensing properties of a-plane ZnO prepared on c-cut sapphire substrate by sputtering

Zinc oxide (ZnO) thin films have been prepared on c-plane sapphire substrate by magnetron sputtering technique. The influence of deposition time on the structural, optical and photoluminescence properties of the films have been investigated. XRD patterns reveal the growth of preferentially oriented (101) non-polar a-plane ZnO film with hexagonal wurtzite structure. The PL peak shifts towards lower wavelength for deposition time up to 20 min, which is in consistent with the results obtained from UV absorption studies. The blue shift in the PL peak confirms the possibility for quantum confinement effect. The band gap energy of the film increases from 3.33 to 3.38 eV, indicating enhanced quantum confinement effects. FESEM micrographs showed that the films have a smooth and dense morphology with uniform grain growth. Hydrogen sensing measurements indicated that a-plane ZnO film on c-sapphire showed higher response than c-plane ZnO film reported earlier. The sensor response of 44 nm thick ZnO film exhibit highest response of 145 towards 500 ppm H₂ gas at the operating temperature of 200 °C.     

超声辅助SILAR法生长纳米晶ZnO多孔薄膜及其光学性能研究

将超声辐照技术引入连续离子层吸附与反应(SILAR)法,提出超声辅助连续离子层吸附与反应(UA-SILAR)液相成膜技术.以锌氨络离子([Zn(NH₃)₄]²⁺)溶液为前驱体,在90℃下沉积得到ZnO薄膜,对其晶体结构,微观形貌、透过光谱和光致发光性能进行表征, 并考察了超声辐照和沉积循环次数对薄膜形貌、结构和光学特性的影响.结果表明,所得薄膜由彼此交联、尺寸均匀的ZnO晶粒组成,呈现典型的多孔特征,同时具有高结晶性和强c轴取向性.由于多孔结构对入射光的散射作用,薄膜在可见光区具有低透射率(约20%);在紫外光激发下,薄膜具有较强的近带边发射和很弱的蓝带发射,体现出薄膜较高的光学质量;薄膜生长过程中超声辐照的引入可对薄膜的结晶性能和微观结构产生显著的影响.     

Optical characterization of ZnO thin films deposited by Sol-gel method

In this paper, ZnO thin film is deposited on Pt/TiO₂/SiO₂/Si substrate using the sol-gel method and the effect of annealing temperature on the structural morphology and optical properties of ZnO thin films is investigated. The ZnO thin films are crystallized by the heat treatment at over 400°C. The ZnO thin film annealed at 600°C exhibits the greatest c-axis orientation and the Full-Width-Half-Maximum (FWHM) of X-ray peak is 0.4360°. A dense ZnO thin film is deposited by the growth of uniform grains with the increase of annealing temperature but when the annealing temperature increases to 700°C, the surface morphology of ZnO thin film becomes worse by the aggregation of ZnO particles. In the results of surface morphology of ZnO thin film using atomic force microscope (AFM), the surface roughness of ZnO thin film annealed at 600°C is smallest, that is, approximately 1.048 nm. For the PL characteristics of ZnO thin film, it is observed that ZnO thin film annealed at 600°C exhibits the greatest UV (ultraviolet) exciton emission at approximately 378 nm, and the smallest visible emission at approximately 510 nm among ZnO thin films annealed at various temperatures. It is deduced that ZnO thin film annealed at 600°C is formed most stoichiometrically, since the visible emission at approximately 510 nm comes from either oxygen vacancies or impurities.     

磁过滤阴极弧制备四面体非晶碳膜热稳定性研究

为研究磁过滤阴极弧制备的四面体非晶碳(tetrahedral amorphous carbon, ta-C)膜在自然环境中使用的热稳定性, 将ta-C膜在空气中退火3h, 退火温度分别为200、400和500℃. 用XPS和Raman谱对膜的微观结构进行表征. 结果表明, 在400及400℃以下退火, XPS谱C1_s峰和Raman谱都没有明显变化. 当退火温度为500℃时, C1_s峰峰形仍然没有变化; Raman峰I_D/I _G增大, G峰峰位未变, 峰的对称性变好. 分析显示膜中石墨颗粒长大, 但没有发生石墨化. 说明磁过滤阴极弧制备的ta-C膜因不含氢和结构致密而表现出良好的热稳定性. 另外, 在退火温度为500℃时, 样品边缘已经氧化挥发.     

Structure, luminescence and electrical properties of ZnO thin films annealed in H2 and H2O ambient: A comparative study

Undoped ZnO films were grown on a c-plane sapphire by plasma-assisted molecular-beam epitaxy technique, and subsequently annealed at 200-500 °C with steps of 100 °C in water vapour and hydrogen ambient, respectively. It is found that the c-axis lattice constant of the ZnO films annealed in hydrogen or water vapour at 200 °C increases sharply, thereafter decreases slowly with increasing annealing temperature ranging from 300 °C to 500 °C. The stress in the as-grown ZnO films was more easily relaxed in water vapour than in hydrogen ambient. Interestingly, the controversial luminescence band at 3.310 eV, which is often observed in photoluminescence (PL) spectra of the ZnO films doped by p-type dopants, was observed in the PL spectra of the annealed undoped ZnO films and the PL intensity increases with increasing annealing temperature, indicating that the 3.310 eV band is not related to p-type doping of ZnO films. The electron concentration of the ZnO films increases sharply with increasing annealing temperature when annealed in hydrogen ambient but decreases slowly when annealed in water vapour. The mechanisms of the effects of annealing ambient on the properties of the ZnO films are discussed.     

连续离子层吸附与反应法(SILAR)生长ZnO多晶薄膜的研究

采用连续离子层吸附与反应法(SILAR),以锌氨络离子([Zn(NH₃)₄]²⁺)为前驱体溶液,在玻璃衬底上沉积了ZnO薄膜,以XRD和SEM等手段分析了薄膜的晶体结构和表面、断面形貌,考察了空气气氛下的退火过程对ZnO薄膜晶体结构与微观形貌的影响,并初步探讨了以SILAR方法沉积ZnO薄膜的机理.结果表明,经200次SILAR沉积循环,所得ZnO薄膜为红锌矿结构的多晶薄膜,沿<002>方向择优生长;薄膜表面致密、光滑均匀,厚度约800nm.退火处理使ZnO薄膜氧缺位减少,晶粒沿c轴取向增强;随退火温度升高,锌间隙原子增加;500℃退火时,ZnO薄膜发生再结晶.减小前驱体溶液的[NH₃·H₂O]/[Zn²⁺]比率可提高ZnO薄膜生长速率.