高温超导薄膜衬底材料LaAlO3单晶的超光滑表面抛光研究

本文以化学机械抛光为手段,以原子力显微镜(AFM)为工具,对高温超导薄膜衬底材料LaAlO3单晶的超光滑表面抛光进行研究.既观察到了由传统光学表面向超光滑表面过渡的过程,又观察到了超光滑表面加工的结果-表面的本征化.显示了超光滑表面抛光对外延衬底表面的重要性.     

中国科学院上海光学精密机械研究所

<正>激光与光电子材料研究发展中心中国科学院上海光学精密机械研究所激光与光电子材料研究发展中心从事晶体材料研究已有40多年的历史,研究方向主要包括:激光晶体、宽禁带半导体衬底晶体、大尺寸蓝宝石晶体、新型发光勺闪烁晶体、光学及光电功能晶体材料等。目前,中心可以提供的主要产品包括:1.激光晶体Ti:Al2O3,Nd:YLF,Nd:YAG,Cr:YAG,Nd:YVO4,Nd,GGG,Yb.YAG,Yb:GSO等;2.高温超导薄膜基片MgO,LaAlO3,SrTiO3,LAST,NdGaO3,YSZ等,3.磁性薄膜与铁电薄膜基片     

(001)高度择优取向Ba0.6Sr0.4TiO3/Pt异质结的结构及性能

采用射频磁控溅射法结合高真空后退火处理,在MgO(001)单晶基片上制备了Pt薄膜.应用脉冲激光沉积法在Pt/MgO上进一步生长了Ba0.6Sr0.4TiO3(BST)薄膜.借助X射线衍射仪(XRD)、铁电测试仪、LCR表研究了BST/Pt/MgO的结构和性能.研究发现,700 ℃真空退火可以保证Pt薄膜在MgO基片上实现(001)高度择优生长,以(001)Pt薄膜为模板,可以进一步获得(001)高度择优取向具有铁电性能BST薄膜.在100 Hz测试频率下,BST薄膜最大介电常数为1100、调谐率为81;、品质因数为21;在7 V的电压下,漏电流密度1.85×10-5 A/cm2,进一步分析表明,BST薄膜在0～2.6 V之间满足欧姆导电机制,在2.6～7 V之间满足普尔-弗兰克导电机制.     

化学机械抛光作用与单晶基片超光滑表面的获取

单晶基片的表面光洁度指标是影响后续薄膜生长质量的重要因素.本文通过对比实验的方法,就采用CMP(chemical mechanical polish)工艺获取超光滑单晶基片做了深入的观察研究,并通过AFM(atomicforce microscope)的最终检测结果给出具有说服力的结论.     

铌酸锂单晶薄膜材料

铌酸锂晶体集电光、声光和非线性光学等物理特性于一身,且透光范围宽,作为一种重要的光学材料被广泛应用于通信、传感等领域。通过离子注入与直接键合的方式制备出的铌酸锂单晶薄膜材料,保留了铌酸锂体材料的优秀物理特性,并且具有高折射率对比度的优点,使光子器件在集成度和性能上都得到了很大程度的提升。本文介绍了铌酸锂薄膜的制备及应用,展示了直径6英寸(1英寸=2.54 cm)的铌酸锂单晶薄膜。将硅单晶薄膜覆盖在铌酸锂单晶薄膜上面,形成一种新型的复合薄膜材料,结合了铌酸锂出色的光学性能和硅出色的电学性能,本文报道了直径3英寸的复合薄膜材料,X射线证明硅薄膜是单晶结构,这种复合薄膜在未来的集成光电芯片中具有应用潜力。     

提拉法制备铜单晶基片的化学机械抛光研究

采用提拉法成功制备出高纯铜(Cu)单晶,最大尺寸为φ15 mm×60 mm.采用化学机械抛光(CMP)方法对Cu单晶基片进行抛光,借助光学显微镜、表面轮廓仪和扫描探针显微镜分析了基片表面形貌、表面粗糙度与表面均匀性,并探讨了抛光压力、表面活性剂和抛光垫对基片表面抛光的影响,结果表明:采用CMP加工后的铜单晶基片表面无宏观划痕、加工均匀性好,基片表面粗糙度Ra为0.921 nm.     

不同应力下的双层钙钛矿锰氧化物La1.3Sr1.7Mn2O7薄膜输运特性研究

采用脉冲激光沉积(PLD)法分别在SrTiO3(100)、LaAlO3 (100)和MgO(100)单晶基片上制备了双层钙钛矿锰氧化物La13Sr17Mn2O7(LSMO)薄膜.X射线衍射谱表明三个样品均沿衬底的晶向择优生长;原子力显微镜显示薄膜表面均光滑致密.采用标准四探针法对薄膜的阻温特性进行了研究,发现SrTiO3 (100)和LaAlO3(100)基片上生长的薄膜呈现出明显的金属-绝缘体转变,转变温度分别为340 K和330 K.而在MgO基片上显示绝缘体态,无金属-绝缘体转变.结合阻温曲线的拟合及薄膜与衬底的晶格失配计算,从薄膜应力和激活能变化的角度分析了样品出现不同阻温特性的内在机制.     

溅射功率对ZnO∶Si透明导电薄膜性能的影响

采用直流磁控溅射法在室温玻璃基片上制备出了掺硅氧化锌(ZnO∶ Si)透明导电薄膜.研究了溅射功率对ZnO∶ Si薄膜结构、形貌、光学及电学性能的影响.结果表明,溅射功率对ZnO∶ Si薄膜的生长速率、结晶质量及电学性能有很大影响,而对其光学性能影响不大.实验制备的ZnO∶Si薄膜为六方纤锌矿结构的多晶薄膜,且具有垂直于基片方向的c轴择优取向.当溅射功率从45 W增加到105 W时,薄膜的晶化程度提高、晶粒尺寸增大,薄膜的电阻率减小;当溅射功率为105 W时,薄膜的电阻率达到最小值3.83×10-4 Ω·cm,其可见光透过率为94.41;.实验制备的ZnO∶ Si薄膜可以用作薄膜太阳能电池和液晶显示器的透明电极.     

双折射雕塑薄膜的研究进展

倾斜沉积技术制备的雕塑薄膜是一种新型的、具有各向异性结构的薄膜材料.根据基片旋转方式的不同,可得到螺旋状、S形状、C形状、弯曲柱状等不同结构的薄膜,并且出现了晶体中的双折射现象.雕塑薄膜可以实现各向同性薄膜无法实现的光学性质,为光学薄膜的设计与制备开辟了新的途径.本文综述了雕塑薄膜的制备方法,分析了雕塑薄膜的微结构与双折射特性,并阐述了其在光学领域内的应用潜力.     

热处理蓝宝石基片对Tl-2212超导薄膜的影响

本文研究了蓝宝石基片的热处理对Tl-2212薄膜的结晶质量、表面形貌及其超导特性的影响.SEM和XRD研究表明,在经过最佳条件(1000 ℃×20 h)退火后的基片上,可以制作出具有致密的晶体结构、高度c轴取向的外延Tl-2212超导薄膜,其薄膜具有优良的电学性能.     

单晶硅低裂纹损伤切片加工技术研究进展

单晶硅晶圆衬底的直径增大、厚度减薄和集成电路(IC)制程减小是集成电路领域主流发展趋势。随着集成电路制程减小至5 nm,对单晶硅晶圆衬底质量的要求越来越高。切片加工是晶圆衬底制造的第一道机械加工工序,金刚石线锯切片是大尺寸单晶硅切片加工的主要技术手段。本文介绍了金刚石线锯切片加工的发展趋势和面临的挑战,阐述了以单晶硅刻划加工研究为基础的金刚石线锯切片加工材料去除机制和电镀金刚石线锯三维形貌建模技术,总结了单晶硅切片加工的晶片表面创成机制和裂纹损伤产生机制,展望了单晶硅低裂纹损伤切片加工的工艺措施,指出了单晶硅切片加工技术的发展趋势,对集成电路制造技术的发展具有一定的指导意义。     

Characterization of lead(II)chloride single crystals grown in silica gel

Acousto‐optical materials play an important role in acousto‐optic devices as acousto‐optic modulators. Lead(II) chloride is an acousto‐optical material, having high figure of merit approximately ten times greater than that of lead molybdate, which is an efficient acousto‐optical material. It also possesses high birefringence, low attenuation coefficient, wide transparency range and good mechanical properties. This paper discusses in detail, the growth of single crystals of lead(II) chloride in silica gel by the process of diffusion in a highly acidic medium. Needle‐type lead(II) chloride crystals have been obtained. The crystal system is confirmed to be orthorhombic by powder X‐ray diffraction analysis. To study the optical transparency of the grown crystal, the transmission spectrum has been recorded in the range 190 – 1100 nm. Thermal stability of the crystal is also studied. Results are discussed in detail. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

钙镁硅酸盐系列结晶釉的研究——钙、镁氧化物对结晶釉析晶的影响

针对钙镁硅酸盐系列结晶釉,研究配方中钙、镁氧化物含量及CaO/MgO比值发生变化时,对釉烧温度及析晶体矿物种属、析晶集合体形态的影响;分析探讨钙、镁氧化物影响析晶的作用机理.研究表明,CaO/MgO比值近于1时,釉烧温度相对较低;CaO/MgO比值向大于1或小于1方向变化时,釉的烧成温度趋于升高.CaO/MgO比值在影响釉析晶体矿物种属的同时,影响析晶集合体的形态特征,认为这是由矿物的析晶习性决定的.     

高温溶液法生长SiC单晶的研究进展

碳化硅(SiC)作为第三代半导体材料,不仅禁带宽度较大,还兼具热导率高、饱和电子漂移速率高、抗辐射性能强、热稳定性和化学稳定性好等优良特性,在高温、高频、高功率电力电子器件和射频器件中有很好的应用潜力。高质量、大尺寸、低成本SiC单晶衬底的制备是实现SiC器件大规模应用的前提。受技术与工艺水平限制,目前SiC单晶衬底供应仍面临缺陷密度高、成品率低和成本高等问题。高温溶液生长(high temperature solution growth, HTSG)法生长SiC单晶具有晶体结晶质量高、易扩径、易实现p型掺杂等独特的优势,有望成为大规模量产SiC单晶的主要方法之一,目前该方法的主流技术模式是顶部籽晶溶液生长(top seeded solution growth, TSSG)法。本文首先回顾总结了TSSG法生长SiC单晶的发展历程,接着介绍和分析了该方法的基本原理和生长过程,然后从晶体生长热力学和动力学两方面总结了该方法的研究进展,并归纳了该方法的优势,最后分析了TSSG法生长SiC单晶技术在未来的研究重点和发展方向。     

高温高压与CVD金刚石单晶衬底质量对比研究

本文通过高分辨X射线衍射(HRXRD)、激光拉曼光谱(Raman)、晶格畸变检测等测试分析方法对多组高温高压(HTHP) Ⅰb、HTHP Ⅱa和化学气相沉积(CVD)型(100)面金刚石单晶样品进行对比研究。HRXRD和Raman的检测结果均表明HTHP Ⅱa型金刚石单晶的结晶质量接近天然金刚石,其XRD摇摆曲线半峰全宽和Raman半峰全宽分别为0.015°~0.018° 和1.45~1.85 cm^-1。晶格畸变检测仪的检测结果表明,HTHP Ⅱa型金刚石单晶的应力分布主要有两种:一种几乎无明显应力分布,另一种沿<110>方向呈对称的放射状分布,其他区域无晶格畸变。HTHP Ⅰb和CVD型金刚石单晶应力分布均相对分散,晶格畸变复杂,与其HRXRD和Raman的检测结果相符。进一步利用等离子体刻蚀法对三种类型金刚石单晶(100)面位错缺陷进行对比分析,结果表明,HTHP Ⅱa型金刚石位错密度为三者中最低,仅为1×10³ cm^-2。本研究为制备高质量大尺寸CVD金刚石单晶的衬底选择提供了实验依据。     

MOVPE homoepitaxy of high-quality GaN: Crystal growth and devices

Epitaxial growth on GaN bulk single crystal substrates sets new standards in GaN material quality. The outstanding properties provide insights into fundamental material parameters (e.g. lattice constants, exciton binding energies, etc.) with a precision not obtainable from heteroepitaxial growth on sapphire or SiC. With metalorganic vapor phase epitaxy (MOVPE) we realized unstrained GaN layers with dislocation densities about six orders of magnitude lower than in heteroepitaxy. By the use of dry etching techniques for surface preparation, an important improvement of crystal quality is achieved. Those layers reveal an exceptional optical quality as determined by a reduction of the low-temperature photoluminescence (PL) linewidth from 5 meV to 0.1 meV and a reduced X-ray diffraction (XRD) rocking curve width from 400 to 20 arcsec. As a consequence of the narrow PL linewidths, new features as, e. g. a fivefold fine structure of the donor-bound exciton line at 3.471 eV was detected. Additionally, all three free excitons as well as their excited states are visible in PL at 2 K.

Dry etching techniques for surface preparation allow morphologies of the layers suitable for device applications. We report on InGaN/GaN multi-quantum-well (MQW)_ structures as well as GaN pn- and InGaN/GaN double heterostructure light emitting diodes (LEDs) on GaN bulk single crystal substrates. Those LEDs are twice as bright as their counterparts grown on sapphire. In addition they reveal an improved high power characteristics, which is attributed to an enhanced crystal quality and an increased p-doping.     

Spray pyrolysis deposition and characterization of highly (100) oriented magnesium oxide thin films

Transparent dielectric thin films of MgO has been deposited on quartz substrates at different temperatures between 400 and 600°C by a pneumatic spray pyrolysis technique using Mg(CH₃COO)₂·4H₂O as a single molecular precursor. The thermal behavior of the precursor magnesium acetate is described in the results of thermogravimetry analysis (TGA) and differential thermal analysis (DTA). The prepared films are reproducible, adherent to the substrate, pinhole free and uniform. Amongst the different spray process parameters, the substrate temperature effect has been optimized for obtaining single crystalline and transparent MgO thin films. The films crystallize in a cubic structure and X‐ray diffraction measurements have shown that the polycrystalline MgO films prepared at 500°C with (100) and (110) orientations are changed to (100) preferred orientation at 600°C. The MgO phase formation was also confirmed with the recorded Fourier Transform Infrared (FTIR) results. The films deposited at 600°C exhibited highest optical transmittivity (>80%) and the direct band gap energy was found to vary from 4.50 to 5.25 eV with a rise in substrate temperature from 500 to 600°C. The measured sheet resistance and the resistivity of the film prepared at 600°C were respectively 10¹³Ω/□ and 2.06x10⁷Ω cm. The surface morphology of the prepared MgO thin films was examined by atomic force microscopy. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

PVT法生长4H-SiC晶体及多型夹杂缺陷研究进展

作为第三代半导体材料的典型代表,碳化硅因具备宽的带隙、高的热导率、高的击穿电场以及大的电子迁移速率等性能优势,被认为是制作高温、高频、高功率以及高压器件的理想材料之一,可有效突破传统硅基功率半导体器件的物理极限,并被誉为带动“新能源革命”的绿色能源器件。作为制造功率器件的核心材料,碳化硅单晶衬底的生长是关键,尤其是单一4H-SiC晶型制备。各晶型体结构之间有着良好的结晶学相容性和接近的形成自由能,导致所生长的碳化硅晶体容易形成多型夹杂缺陷并严重影响器件性能。为此,本文首先概述了物理气相传输(PVT)法制备碳化硅晶体的基本原理、生长过程以及存在的问题,然后针对多型夹杂缺陷的产生给出了可能的诱导因素并对相关机理进行解释,进一步介绍了常见的碳化硅晶型结构鉴别方式,最后对碳化硅晶体研究作出展望。     

Growth and characterization of a novel NLO crystal bis-glycine hydrogen chloride (BGHC)

Single crystals of bis-glycine hydrogen chloride (BGHC), a semiorganic nonlinear optical (NLO) material, have been grown by slow solvent evaporation technique. Good optical quality single crystals with dimensions up to 33×5×5 mm³ are obtained. The crystals are characterized by optical transmission spectrum, FTIR and X-ray diffraction studies. The thermal stability of the crystal is studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The second harmonic generation (SHG) efficiency of BGHC was found to be 5.6 times that of KDP. The laser damage threshold values studied in single shot mode indicates that BGHC crystal possesses a fairly high value of 9.8 GW/cm² and thus the NLO studies confirmed the superiority of BGHC over KDP and urea crystals. The dielectric constant of the crystal was studied as a function of frequency and the results are discussed.     

Substrate effect on microstructure and optical performance of sputter‐deposited TiO2 thin films

This study deals with the role of the different substrates on the microstructural, optical and electronical properties of TiO₂ thin films produced by conventional direct current (DC) magnetron sputtering in a mixture of pure argon and oxygen using a Ti metal target with the aid of X–ray diffractometer (XRD), ultra violet spectrometer (UV–vis) and atomic force microscopy (AFM) measurements. Transparent TiO₂ thin films are deposited on Soda lime glass, MgO(100), quartz and sitall substrates. Phase purity, surface morphology, optical and photocatalytic properties of the films are compared with each other. It is found that the amplitude of interference oscillation of the films is in a range of 77‐89%. The transmittance of the film deposited on Soda lime glass is the smallest while the film produced on MgO(100) substrate obtains the maximum transmittance value. The refractive index and optical band gap of the TiO₂ thin films are also inferred from the transmittance spectra. The results show that the film deposited on Soda lime glass has the better optical property while the film produced on MgO(100) substrate exhibits much better photoactivity than the other films because of the large optical energy band gap. As for the XRD results, the film prepared on MgO(100) substrate contains the anatase phase only; on the other hand, the other films contain both anatase and rutile phases. Furthermore, AFM images show that the regular structures are observed on the surface of all the films studied. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)