生长气压对分子束外延β-Ga2O3薄膜特性的影响

本文采用分子束外延技术在具有6°斜切角的c面蓝宝石衬底上外延β-Ga₂O₃薄膜,系统研究了生长气压对薄膜特性的影响。X射线衍射谱和表面形貌分析表明,不同生长气压下所外延的薄膜表面平整,均具有(201)择优取向。并且,其结晶质量和生长速率均随生长气压增大而逐渐提高。通过X射线光电子能谱分析发现,生长气压增大使得氧空位的浓度大幅下降,高价态Ga比例增大,最终使得O/Ga原子数之比接近理想Ga₂O₃材料的化学计量比值。利用Tauc公式和乌尔巴赫带尾模型进行计算,结果表明随着生长气压的增大,样品的光学带隙由4.94 eV增加到5.00 eV,乌尔巴赫能量由0.47 eV下降到0.32 eV,证明了生长气压的增大有利于降低薄膜中的缺陷密度,提高薄膜晶体质量。     

不同退火条件对PEALD制备的Ga2O3薄膜特性的影响

利用等离子增强原子层沉积技术(PEALD)在c面蓝宝石衬底上制备了氧化镓(Ga₂O₃)薄膜,研究了退火气氛(v(N₂)∶v(O₂)=1∶1(体积比)、空气和N₂)及退火时间对Ga₂O₃薄膜晶体结构、表面形貌和光学性质的影响。研究结果表明,退火前的氧化镓处于亚稳态,不同退火气氛下退火后晶体结构发生明显改变,而且退火气氛中N₂比例增加有利于Ga₂O₃重结晶。在N₂气氛下退火达到30 min,薄膜结构已由亚稳态转变成择优取向的β-Ga₂O₃。而且表面形貌分析表明,退火30 min后表面形貌开始趋于稳定,表面晶粒密度不再增加。另外实验样品在 400~800 nm的平均透射率几乎是100%,且光吸收边陡峭。采用N₂气氛退火,对于富氧环境下沉积的Ga₂O₃更利于薄膜表面原子迁移,以及择优取向Ga₂O₃重结晶。     

雾化辅助化学气相沉积法氧化镓薄膜生长研究

采用自主设计搭建的雾化辅助化学气相沉积系统设备,开展了Ga₂O₃薄膜制备及其特性研究工作。通过X射线衍射研究了沉积温度、系统沉积压差对Ga₂O₃薄膜结晶质量的影响。结果表明,Ga₂O₃在425~650 ℃温度区间存在物相转换关系。随着沉积温度从425 ℃升高至650 ℃,薄膜结晶分别由非晶态、纯α-Ga₂O₃结晶状态向α-Ga₂O₃、β-Ga₂O₃两相混合结晶状态改变。通过原子力显微镜表征探究了生长温度对Ga₂O₃薄膜表面形貌的影响,从475 ℃升高至650 ℃时,薄膜表面粗糙度由26.8 nm下降至24.8 nm。同时,高分辨X射线衍射仪测试表明475 ℃、5 Pa压差条件下的α-Ga₂O₃薄膜样品半峰全宽仅为190.8″,为高度结晶态的单晶α-Ga₂O₃薄膜材料。     

不同退火温度对钡铁氧体薄膜磁性的影响

M型钡铁氧体(BaFe₁₂O₁₉, BaM)是一种单轴磁晶各向异性的六角晶系硬磁材料,由于其具有很强的各向异性场,因此在自偏置微波器件领域具有广阔的应用前景。本文采用常温射频磁控溅射法在(000l)取向的蓝宝石衬底上沉积了厚度约为130 nm的BaFe₁₂O₁₉非晶薄膜,然后分别在850 ℃、900 ℃、950 ℃、1 000 ℃对其空气退火处理3 h,得到BaM晶体薄膜样品。采用X射线衍射仪对薄膜样品进行物相及晶体生长取向鉴别,采用扫描探针显微镜和扫描电子显微镜对薄膜样品的粗糙度和表面形貌进行测量和观察,采用振动样品磁强计对样品进行了静态磁性能测试。实验结果表明,退火后的薄膜样品的主晶相为BaM,且具有(000l)取向择优生长,其微观组织结构都表现为C轴垂直于膜面的颗粒状结构。退火温度为900 ℃时所得样品的各项性能达到最佳,其表面粗糙度为2.8 nm,矩形比为0.84,饱和磁化强度为247 emu/cm³,矫顽力为1 528 Oe。     

磁控溅射衬底加热温度和后退火温度对制备β-Ga2O3薄膜材料的影响

作为宽禁带半导体材料的一员,结构稳定的β-Ga₂O₃具有比SiC和GaN更宽的禁带宽度和更高的巴利加优值,近年来受到科研人员的广泛关注。本文采用射频(RF)磁控溅射法在C面蓝宝石衬底上生长β-Ga₂O₃薄膜,探究溅射过程中衬底加热温度的影响。溅射完成后通过高温退火处理提升薄膜质量,研究衬底加热温度和后退火温度对氧化镓薄膜晶体结构和表面形貌的影响。利用X射线衍射(XRD)、原子力显微镜(AFM)等测试手段对β-Ga₂O₃薄膜晶体结构、表面形貌等进行分析表征。实验结果表明,随着衬底加热温度的升高,β-Ga₂O₃薄膜表面粗糙度逐渐降低,薄膜晶体质量得到显著提升;在氧气气氛中进行后退火,合适的后退火温度有利于氧化镓薄膜重新结晶、增大晶粒尺寸,能够有效修复薄膜的表面态和点缺陷,对于改善薄膜晶体质量有明显优势。     

压电晶体YbBa3(PO4)3的生长与性质表征

压电材料在振动传感器、压力传感器和超声波压电换能器等器件技术领域有着广泛应用,探索新型压电晶体材料用于特种压电传感器件的研发具有重要意义。本文利用传统的提拉法生长出具有高熔点(~1 800 ℃)的磷酸钡镱(YbBa₃(PO₄)₃,YbBP)新型压电晶体。X射线衍射分析表明,该晶体属于立方晶系I43d空间群,晶胞参数为a=b=c=1.043 5 nm。研究发现,该晶体沿垂直于(013)晶面的方向更容易生长。摇摆曲线半峰全宽测得为60.6″,表明生长的晶体具有较高的结晶品质。采用LCR电桥法、阻抗法和超声法测算了该晶体的相对介电常数和压电应变常数,得到晶体的相对介电常数ε₁₁和压电应变常数d₁₄分别为15.3和11.4 pC/N。该晶体不仅具有较好的压电性能,同时具有纯的面切变振动模态,表明该晶体在压电传感技术领域具有潜在应用。     

KCaCl3:Ce晶体的生长及发光性能

采用坩埚下降法生长出不同摩尔分数Ce³⁺(1%、2%、4%、6%、8%)掺杂的KCaCl₃:Ce单晶。晶体属于正交晶系,晶胞参数为a=0.756 0 nm,b=1.048 2 nm,c=0.726 6 nm。热重分析仪测得熔点为740 ℃,透过率测试显示晶体在可见光波段均具有较好光学透过率。对晶体的光致发光光谱、光致衰减时间、X射线激发发射光谱、透过率等光学性能进行了表征。光致发光光谱显示KCaCl₃:Ce晶体在358 nm和378 nm波长左右有宽的发射峰,符合Ce³⁺的5d₁→²F_5/2和5d₁→²F_7/2能级跃迁,通过拟合,KCaCl₃:Ce晶体的衰减时间在30 ns左右。晶体在X射线激发下均表现出优异的X射线发光性能。     

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%。     

溅射温度对ITO/Ag/ITO多层复合薄膜的结构和光电性能的影响

本文采用直流磁控溅射分层溅射制备了氧化铟锡(ITO)/银(Ag)/ITO多层复合薄膜。系统研究了溅射温度对ITO/Ag/ITO多层复合薄膜的结构和光电性能影响。采用ITO(m(In₂O₃)∶m(SnO₂)=9∶1;直径60 mm)靶材和Ag(纯度99.999%;直径60 mm)靶材分层溅射,使ITO薄膜和Ag薄膜依次沉积在钠-钙玻璃基片上。结果表明,溅射温度对该薄膜的形貌和结构具有显著的影响。在中间Ag薄膜和顶层ITO薄膜的溅射温度均为120 ℃时,薄膜表面晶粒形貌由类球形转变为菱形,此时薄膜方阻为3.68 Ω/Sq,在488 nm处透射率为88.98%,且品质因数为0.03 Ω^-1,实现了低方阻高可见光透射率ITO/Ag/ITO多层复合薄膜的制备。     

Cs3Bi2I9晶体的生长及辐射探测性能

采用布里奇曼法成功制备出大尺寸(φ15 mm×50 mm)、高质量的全无机金属卤化物类钙钛矿Cs₃Bi₂I₉单晶。室温下,该晶体属于六方晶系,空间群为P6₃/mmc,密度为5.07 g/cm³,晶胞参数为a=b=0.840 nm,c=2.107 nm,熔点为632 ℃。采用粉末X射线衍射谱、紫外-可见-近红外漫反射光谱、I-V测试等表征该晶体的性质。制备Au/Cs₃Bi₂I₉/Au三明治型器件结构,采用飞行时间技术测试Cs₃Bi₂I₉晶体的载流子迁移率,得到Cs₃Bi₂I₉晶体的电子迁移率为4.33 cm²·V^-1·s^-1。根据Hecht单载流子方程拟合得到Cs₃Bi₂I₉晶体的载流子迁移率寿命积(μτ)为8.21×10^-5 cm²·V^-1,并且在500 V偏压下对α粒子的能量分辨率达到39%。     

Formation of LiNbO3 films by hydrolysis of metal alkoxides

Homogeneous, crack-free, thin films of crystalline LiNbO₃ were synthesized above 250°C on Si(100) substrates by the dip-coating method using a double alkoxide solution. The coating solution, which was prepared by the controlled partial hydrolysis of the double alkoxide, gave stoichiometric LiNbO₃ crystalline films at temperatures as low as 250°C. The concentration of the alkoxide solution influenced both of thickness and quality of films. Crystallinity of thin film top-coated directly on the substrate affected the crystallization state of films coated on the film remarkably. Films crystallized on -Al₂O₃(0001) showed preferred orientation along the c-axis, while the preferred orientation could not be observed on Si(100) substrates.     

Correlation between interfacial structure and c-axis-orientation of LiNbO3 films grown on Si and SiO2 by electron cyclotron resonance plasma sputtering

Thin films of crystalline lithium niobate (LN) grown on Si(1 0 0) and SiO₂ substrates by electron cyclotron resonance plasma sputtering exhibit distinct interfacial structures that strongly affect the orientation of respective films. Growth at 460–600 °C on the Si(1 0 0) surface produced columnar domains of LiNbO₃ with well-oriented c-axes, i.e., normal to the surface. When the SiO₂ substrate was similarly exposed to plasma at temperatures above 500 °C, however, increased diffusion of Li and Nb atoms into the SiO₂ film was seen and this led to an LN–SiO₂ alloy interface in which crystal-axis orientations were randomized. This problem was solved by solid-phase crystallization of the deposited film of amorphous LN; the degree of c-axis orientation was then immune to the choice of substrate material.     

钴酸钙薄膜的制备及高温吸波性能研究

以溶胶凝胶法制备的钴酸钙粉体为基础材料,在氧化铝陶瓷基板上涂覆烧结形成了钴酸钙薄膜,研究了薄膜的物相结构、温阻特性及电磁波吸收性能。研究发现,溶胶凝胶法制备的钴酸钙粉体由Ca₉Co₁₂O₂₈相组成,粉体颗粒均匀,具有一定的取向性生长,呈明显的片层状结构。烧结后的钴酸钙薄膜由细小的Ca₃Co₄O₉相组成,与氧化铝基板结合紧密,厚度在20 μm左右,薄膜的方阻值随着温度的升高迅速下降,在300~800 ℃保持在20 Ω/□左右。800 ℃钴酸钙电阻膜型超材料吸波体在8~18 GHz显示出了对电磁波双吸收峰特征。     

Analysis of the growth of RF sputtered ZnO thin films using the optical reflective second harmonic generation

Reflective second harmonic generation (RSHG) is used to analyze the growth condition of poly crystal zinc oxide (ZnO) film with a c-axis orientation, grown on the Si substrate by RF magnetron sputtering technique. It elucidates physical phenomena exhibited by growing ZnO thin films. Connecting with analytical results of the characteristic parameters derived from the X-ray patterns and SEM images, the relationship between the RSHG intensity and the substrate temperature reveals that the effect of the grain boundaries is the domination of the RSHG mechanism. The inclined structures of ZnO films on the Si substrate are explained with reference to these RSHG patterns.     

High-resolution XRD study of stress-modulated YBCO films with various thicknesses

High-quality epitaxial YBa₂Cu₃O_7−δ (YBCO) superconducting films with thicknesses between 0.2 and 2 μm were fabricated on (0 0 l) LaAlO₃ with direct-current sputtering method. The influence of film thickness on the structure and texture was investigated by X-ray diffraction conventional θ–2θ scan and high-resolution reciprocal space mapping (HR-RSM). The films grew with strictly c-axis epitaxial, and no a-axis-oriented growth was observed up to a thickness of 2 μm. Lattice parameters of the YBCO films with different thicknesses were extracted from symmetry and asymmetry HR-RSMs. The X-ray lattice parameter method was used to determine the residual stress in YBCO films by measuring the a-, b-, c-axis strains, respectively. The results showed that YBCO films within thinner than 1 μm were under compressive stress, which was relieved increasing of film thickness. However, beyond 1 μm in thickness, YBCO films exhibited a tensile stress. Based on the experimental analysis, the variety of residual stresses in the films is mainly attributed to oxygen vacancies with thickness of YBCO film increasing.     

Epitaxial growth of CuInSe2 single crystal by halogen transport method

CuInSe₂ single crystals were epitaxially grown on (001) GaP, (001) GaAs, and (110) GaP by the halogen transport method. The orientation relationships in the growth on the (001) and (110) faces were (a) [001]_CuInSe2 [001]_sub and [100]_CuInSe2 [100]_sub (c-axis orientation growth), and (b) [110]_CuInSe2 [110]_sub and [001]_CuInSe2 [001]_sub, respectively. On (001) InP, the orientation relationships between the layer and substrate consist of two sets: (c) [100]_CuInSe2 [001]_sub and [001]_CuInSe2 [010]_sub, and (d) [100]_CuInSe2 [001]_sub and [001]_CuInSe2 [ 00]_sub (a-axis orientation growth). The above results, i.e., c-axis growth on (001) GaP and (001) GaAs and a-axis growth on (001) InP, could be explained by a criterion of the minimum lattice mismatch between grown layers and substrates. A series of growth experiments on (001) GaAs indicated that appropriate gas etching of the substrate surface and growth temperature were required for obtaining twin-free single-crystal epitaxial CuInSe₂.