电子束蒸发制备PbI2膜及其光学性能研究

采用电子束蒸发法制备PbI2膜,研究不同工艺参数对制备样品光学性质的影响.结果表明,制备样品属于六方相多晶结构,随衬底温度的升高,样品中的I元素含量降低并趋于理想化学配比.随着衬底温度的升高,PbI2膜的光谱透过性能逐渐改善,吸收边沿低能一侧的拖尾逐步消除,源自样品结晶质量的提高.根据紫外-可见透过谱,计算了不同条件下制备样品的厚度、折射率、吸收系数和光学带隙.结果发现,随衬底温度的升高,制备样品的折射率和光学带隙出现波动变化,但吸收系数单调增大.在相同的衬底温度下,35 cm的源-衬间距下制备的样品具有最大的光吸收系数,归因于该系列样品较高的致密度.     

衬底温度对电子束蒸发ZnS薄膜结构和光学特性的影响

采用电子束蒸发法在不同衬底温度下,150℃、200℃、250℃和300℃,制备了ZnS薄膜;用X射线衍射仪、原子力显微镜、膜厚仪和紫外-可见光-近红外分光光度计分别表征ZnS薄膜的晶体结构、表面形貌和光学特性;并分析了不同衬底温度对薄膜的结构和光学特性的影响.结果表明:在硅衬底上制备的ZnS都为多晶薄膜,具有闪锌矿β-ZnS结构;随衬底温度升高呈(111)晶面高度择优取向,平均晶粒尺寸有所增大,内应力、位错密度、折射率和吸收系数有所减小,禁带宽度随之增大;衬底温度为300℃时制备的薄膜表面均匀致密,呈现较优的结构和光学性能.     

退火温度对La3Ga5SiO14薄膜结构及表面形貌的影响

采用脉冲激光沉积技术在Si(100)衬底上制备了La3Ga5SiO14薄膜,并研究了不同的退火温度对薄膜结构和表面形貌的影响.衬底温度为室温时生长的薄膜经过800 ℃以上的高温退火后,由最初的无定形态转变为无规则取向的多晶结构.衬底温度为400 ℃时生长的薄膜经过800 ℃退火处理后呈现无序的多晶形态.当退火温度进一步升高至1000 ℃时,XRD图谱显示薄膜由最初的(220)和(300)两个结晶方向转变为以(200)和(400)为主要取向的多晶结构.表面形貌分析表明:衬底温度为400 ℃时,随着退火温度的升高,薄膜颗粒尺寸逐渐增大,表面无裂纹,而衬底温度为室温时生长的薄膜退火后则出现大量的裂缝、孔洞等缺陷.     

不同衬底表面上大晶粒多晶Si薄膜的制备

利用高频感应加热化学气相沉积(HFCVD)工艺,以H2稀释的SiH4作为反应气体源,分别在n-(111)Si衬底上常规热生长的SiO2层、织构的SiO2层和纳米晶粒多晶Si薄膜表面上,制备了具有均匀分布的大晶粒多晶Si膜.采用扫描电子显微镜(SEM)和X射线衍射(XRD)等检测手段,测量和分析了沉积膜层的表面形貌、晶粒尺寸、密度分布与择优取向等结构特征.结果表明,多晶Si膜中Si晶粒的尺寸大小和密度分布不仅与衬底温度、SiH4浓度与反应气压等工艺参数有关,而且强烈依赖于衬底的表面状态.本实验获得的最好的薄膜中,Si晶粒平均尺寸约为2.3 μm,密度分布约为3.8×107/cm2.对薄膜的沉积机理分析表明,衬底表面上Si原子基团的吸附、迁移、成核与融合等热力学过程支配着大晶粒多晶Si膜的生长.     

衬底温度对共蒸发制备GaSb多晶薄膜性质的影响

采用共蒸发的方法在玻璃衬底上制备出GaSb多晶薄膜材料.研究了薄膜生长速率与衬底温度、Ga源温度和Sb源温度的关系.通过XRD、UV-Vis、Hall效应和AFM等测试方法,研究了衬底温度对于GaSb薄膜的结构特性、光电性质以及表面形貌的影响.GaSb多晶薄膜具有(111)择优取向,薄膜的吸收系数达到105 cm-1,晶粒尺寸随衬底温度升高逐渐增大;衬底温度为540℃时,薄膜的迁移率达到127 cm2/V·s,空穴浓度为3×1017 cm-3.GaSb薄膜的表面粗糙度随温度增加而增加.     

纯氮气反应溅射AlN薄膜及性质研究

在不同氮气浓度、不同溅射气压和衬底温度为20～370 ℃的条件下,分别在多种衬底上采用反应磁控溅射法沉积AlN薄膜.X射线衍射图谱表明:温度大于180 ℃时可在多种衬底上沉积出具有c轴择优取向的纤锌矿AlN薄膜.衬底温度和溅射时间的增加有利于薄膜结晶性的改善. 1.5 Pa的纯氮气气氛和Si(100)衬底是最佳择优生长条件.由紫外-可见光透射谱计算得到:在石英衬底上沉积的薄膜折射率为1.80～1.85,膜厚约为 1 μm、光学能隙为6.1 eV.原子力显微镜照片表明:在Si(100)衬底上制备的薄膜表面平滑,均方根粗糙度为2.2～13.2 nm.     

纳米晶粒多晶Si薄膜的低压化学气相沉积

利用低压化学气相沉积(LPCVD)方法,以充Ar的SiH4作为反应气体源,在覆盖有热生长SiO2层的p-(100)Si衬底上制备了具有均匀分布的纳米晶粒多晶Si膜(nc-poly-Si).采用扫描电子显微镜(SEM)、原子力显微镜(AFM)和拉曼谱等检测手段,测量和分析了沉积膜层的表面形貌、晶粒尺寸与密度分布等结构特征.结果表明,nc-poly-v膜中Si晶粒的尺寸大小和密度分布强烈依赖于衬底温度、SiH4浓度与反应气压等工艺参数.典型实验条件下生长的Si纳米晶粒形状为半球状,晶粒尺寸约为40nm,密度分布约为4.0×1010cm-2和膜层厚度约为200nm.膜层的沉积机理分析指出,衬底表面上Si原子基团的吸附、迁移、成核与融合等热力学过程支配着nc-poly-Si膜的生长.     

SiC衬底上β-Ga2O3薄膜生长及p-SiC/n-β-Ga2O3异质结光伏特性

本文采用脉冲激光沉积(PLD)技术在p型4H-SiC衬底上,制备出沿(403)择优生长的β-Ga₂O₃薄膜。结果表明,衬底生长温度对β-Ga₂O₃薄膜的形貌、结构、组分,以及生长机理都有重要影响。当生长温度由300 ℃升高至500 ℃时,薄膜结晶质量随生长温度升高而提高,当温度进一步升高到600 ℃时,薄膜结晶质量变差,这是由于在相对低温(500 ℃以下)阶段,生长温度越高,沉积在衬底上原子的动能越大,越容易迁移,使得β-Ga₂O₃薄膜主要按照二维生长模式进行生长,薄膜结晶质量提高,表现为随着生长温度升高,粗糙度降低。但当温度上升到600 ℃时,由于4H-SiC衬底和β-Ga₂O₃薄膜之间的热膨胀系数存在差异,导致薄膜生长由主要以二维生长模式向三维岛状演变。基于p-4H-SiC/n-β-Ga₂O₃构筑的异质结太阳电池,其标准测试条件下光电转换效率达到3.43%。     

双靶磁控溅射聚焦共沉积AlN薄膜生长速率研究

采用直流双靶磁控溅射聚焦共沉积技术在Fe衬底上高速率生长A lN薄膜,结果表明,双靶共沉积技术有效地提高了A lN薄膜生长速率,相同工作气压或低N2浓度时双靶磁控溅射沉积速率约为单靶沉积速率的2倍;随着溅射系统内工作气压或N2浓度的升高,薄膜生长速率不断减小;薄膜择优取向与薄膜生长速率相互影响,随着工作气压的升高,(100)晶面的择优生长减缓了薄膜生长速率的降低,随着N2浓度的升高,(002)晶面的择优生长加剧了薄膜生长速率的降低,而相对较低的溅射沉积速率有利于(002)晶面择优取向生长。     

CdS多晶薄膜的制备与光学性质研究

采用电子束蒸发法制备CdS多晶薄膜,研究了衬底温度和退火方式对薄膜光学性质的影响。XRD测试显示,制备样品为六方相多晶结构,沿(002)晶向择优取向生长,在200℃衬底温度时具有最大的择优取向度。对样品的紫外-可见透过谱测试表明,随着衬底温度的升高,薄膜的光吸收边逐渐变陡,光学带隙逐渐增大。退火后,CdS薄膜光吸收边变的更加陡直,光谱透过性能进一步提升,但光学带隙变化很小。此外,制备样品的XRD谱、光吸收边和光学带隙在250℃衬底温度下出现反常变化。同时对上述变化产生的根源进行了分析和讨论。     

MgO(100)衬底上生长BaTi2O5薄膜及其性能研究

利用脉冲激光沉积技术,在MgO(100)衬底上生长了BaTi2O5薄膜,探讨了沉积条件(衬底温度和氧分压)对薄膜结构的影响,并对其介电和光学性能进行了研究.结果表明:随衬底温度和氧分压的改变,BaTi2O5薄膜的物相和结晶取向逐渐变化;适宜的脉冲激光沉积工艺为衬底温度950~1000 K、氧分压12.5 Pa,在该条件下获得了b轴方向择优生长的BaTi2O5薄膜;该薄膜具有较高的居里温度(750 K),介电常数达2000,而且在可见光和红外波长范围内具有较高的透过率.     

衬底温度对氧化锌薄膜微结构及光学性能的影响

衬底温度是磁控溅射法制备氧化锌薄膜中一个非常重要的工艺指标,探索衬底温度对氧化锌薄膜微结构及光学性能的影响对制备环保型高质量氧化锌紫外屏蔽材料具有重要意义。以质量分数99.99%的氧化锌陶瓷靶为溅射源,利用射频磁控溅射技术在石英衬底上沉积了氧化锌紫外屏蔽薄膜,通过X射线衍射仪、薄膜测厚仪、紫外-可见分光光度计、荧光分光光度计进行测试和表征,研究了不同衬底温度对ZnO薄膜微结构及光学性能的影响。实验结果表明:制备所得薄膜均为六角纤锌矿结构,具有沿(002)晶面择优取向生长的特点,其晶格常数、晶粒尺寸、透过率、光学能隙、可见荧光、结晶质量等都与衬底温度密切相关,当衬底温度为250 ℃,溅射功率160 W,氩气压强0.5 Pa,氩气流速8.3 mL/min,沉积时间60 min时,所得氧化锌薄膜样品取向性最好,晶粒尺寸最大,薄膜结构致密,具有良好的光学性能和结晶质量。     

衬底温度对Cu2O薄膜结构和性能的影响

采用射频磁控溅射技术在石英衬底上制备了Cu2O薄膜。系统研究了衬底温度对薄膜结构、光学和电学性能的影响。XRD的结果显示,在所有衬底温度条件下均可得到单相的Cu2O结构,而且随着衬底温度由500 K升至800 K,薄膜表现出(111)择优取向的生长特点。电学和光学测试结果表明,室温电导率和光学带隙随着衬底温度的升高而增加,800 K制备的薄膜的带隙值最高约为2.58 eV。     

高硼硅玻璃薄膜的磁控溅射沉积及性能研究

本文采用射频磁控溅射法,以高硼硅玻璃为靶材,在高硼硅玻璃基底上制备高硼硅玻璃薄膜。探讨磁控溅射法与熔融法制得的高硼硅玻璃的性能差异,研究磁控溅射功率对高硼硅玻璃薄膜质量的影响。通过X射线衍射仪(XRD)、傅里叶红外光谱仪(FT-IR)、X射线光电子能谱仪(XPS)、扫描电镜(SEM)、台阶仪、紫外可见(UV-Vis)分光光度计和纳米压痕仪器等对薄膜的物相结构、成分、沉积速率、透光率,以及纳米硬度和杨氏模量进行表征与分析。结果表明:本实验所制备的高硼硅玻璃薄膜为非晶态结构;当工作气压为0.6 Pa时,薄膜的沉积速率随溅射功率上升不断增加;对比不同溅射功率下的透光率,发现高硼硅玻璃薄膜对基体的透光性影响较小,当溅射功率为150 W,可见光透光率损失仅为2%;不同溅射功率下获得薄膜的纳米硬度和杨氏模量随溅射功率先增大后减小,在120 W时达到最大峰值,相较于原玻璃基底分别提升3%和3.5%。     

钙钛矿太阳能电池的制备工艺与光伏性能研究

设计和制备结构为FTO玻璃/TiO2致密层/TiO2介孔层/CH3NH3PbI3吸收层/C电极的钙钛矿太阳能电池.采用两步法制备CH3NH3PbI3吸收层:首先通过旋涂技术制备PbI2薄膜,然后将PbI2薄膜在浓度为0.044 mol/L的甲基碘化胺/异丙醇(MAI/IPA)溶液中分别浸泡反应0.5 h、2.5 h、3.5 h和4.0 h后获得CH3NH3PbI3吸收层.研究了浸泡反应时间对CH3NH3PbI3吸收层的结构和形貌以及对电池光伏性能的影响.结果表明:PbI2薄膜在MAI/IPA溶液中反应后形成四方结构的CH3NH3PbI3晶粒,当浸泡反应3.5 h时,CH3NH3PbI3晶粒的平均尺寸最大,均匀性较好;XRD图谱中只有CH3NH3PbI3的特征峰,而PbI2的特征峰完全消失.同时,该条件下制备的钙钛矿太阳能电池的光伏性能最佳,其开路电压0.881 V、短路电流密度达到22.17 mA/cm2,光电转化效率6.79;,且在整个可见光区的光子-电子的转换效率接近50;.     

Photocatalytic TiO2 films prepared by chemical vapor deposition at atmosphere pressure

Nanometer semiconductor titanium dioxide thin films have excellent properties of photocatalysitic degeneration. The glass coated TiO₂ films is called self-cleaning glass. In this paper, chemical vapor deposition (CVD) method is employed to deposit TiO₂ films on glass. The effect of spacing between nozzle and glass and the effect of substrate temperature on deposition rate are studied. The crystalline structure at different deposition temperatures is analyzed by XRD and anatase was found. And the microstructure of the TiO₂ films is also determined by SEM. It shows that the size of crystal grain increases with the temperature.     

Crystallographic defects in epitaxial layers of cadmium sulphide

Thin epitaxial films of CdS deposited in high vacuum on ionic single crystal substrates have been studied by transmission electron microscopy. The (100), (110) and (111) faces of NaCl and the (111) face of BaF₂ were used as substrate surfaces. Both cubic sphalerite and hexagonal wurtzite structure films have been produced. The orientations of the sphalerite structure films were (100) and (110) and were produced on substrate faces having the same two orientations. The wurtzite structure films were in (0001) orientation and grew on (111) oriented substrate faces. For a fixed rate of deposition both the number and type of defects found in the films appear to be dependent upon the growth temperature and the crystal structure. Annealing the films at a high temperature has been tested as a means for reducing their defect content and the effect is very different for the two crystal structures. A reduction in the defect content of the wurtzite structure films is induced but no change in the crystal structure occurs. In contrast to this, the sphalerite structure films undergo a progressive phase transformation to the wurtzite stucture while at the same time losing a high proportion of their defects.     

单晶MgO基片超精密加工技术研究

单晶MgO具有良好的物理化学性能及光学性能,是性能优异的薄膜基片及光学零件材料,广泛应用于高温超导、航空航天、光电技术等领域.用作薄膜生长的基片必须具有高精度超光滑无损伤的表面,而单晶MgO是典型的硬脆难加工材料,这对MgO晶体的超精密加工技术提出了很高的要求.本文介绍了单晶MgO的特性及其应用领域,针对高温超导薄膜制备对MgO基片的要求,讨论了现有的MgO基片加工工艺存在的问题,分析了几种可用于MgO基片超精密加工的先进工艺技术的特点和应用研究现状.     

A Polymorph Crystal Structure of Hexaphenyl Observed in Thin Films

Highly oriented thin films of hexaphenyl — which are used in organic opto‐electronic applications — are characterised in terms of their crystal structures. Two different crystal structures of hexaphenyl (C₃₆H₂₆) are observed when the films are prepared by physical vapour deposition at various substrate temperatures. If the substrate is kept at room temperature, hexaphenyl crystallises within a structure which is already known from single crystal investigations. However, when the thin films are grown at a substrate temperature of 160°C a new crystalline phase appears. This structure was characterised by X‐ray and transmission electron diffraction. Due to the strong preferred orientation of the crystallites within the thin films, the lattice constants as well as main features of the new crystal structure could be determined. The lattice is indexed as monoclinic with: a = 7.98Å, b = 5.54Å, c = 27.64Å and β = 99.8°. The new crystal structure has high similarity to the already known crystal structure: Both structures are built by layers of hexaphenyl molecules, within one layer the aromatic planes of the hexaphenyl molecules are packed in a herringbone pattern. The characteristic feature of the new structure is that the long axes of the hexaphenyl molecules are arranged absolutely perpendicular to the layers, whereas, within the already known structure the long axes show an tilt angle of 17° to the layer normal direction.     

Deposition of microcrystalline Ge films using hot-wire technique without toxic gases

To investigate the deposition of Ge films without toxic gas such as germane, we have studied the Ge films prepared by the hot-wire technique, which utilize the reaction between a Ge target and hydrogen atoms generated by the hot-wire decomposition of H₂ gas. The films deposited on Si substrate were microcrystalline Ge films and the mean crystallite size of the films increased from 13.3 to 24.8 nm with increasing the substrate temperature from 300 to 500 °C. Moreover, the deposition rate of Ge films deposited on Si substrate was higher than that of Ge films deposited on Corning 1737 substrate. It was found that the substrate temperature and the kind of substrate are key parameters for the preparation of microcrystalline Ge films by the hot-wire technique.