Assessment of mismatched epitaxial layers by X-ray rocking curve measurements and simulations

In the design of heteroepitaxial systems the knowledge of composition, strain and thickness of the various layers involved is of great importance. The determination of these structural parameters is among the applications most common in high-resolution X-ray diffraction. Numerical simulation of rocking curves has emerged as an important aid in the determination of the relevant structural parameters. Based upon the dynamical theory of X-ray diffraction a FORTRAN program has been written to simulate and refine structural parameters from rocking curve data. X-ray rocking curve analysis has been used to develop and optimize MOCVD-growth of Ga_xIn_1-xP/GaAs heteroepitaxial systems. We observed superlattice peaks in samples of low misfit. With the aid of computer simulations we attribute these to unintentional periodic compositional fluctuations (Ga/In) of the order of 1%.     

InGaP/GaAs heterojunction bipolar transistor grown by solid-source molecular beam epitaxy with a GaP decomposition source

Lattice-matched InGaP epilayers on GaAs (001) and InGaP/GaAs heterojunction bipolar transistors (HBTs) were successfully grown by solid-source molecular beam epitaxy (SSMBE) with a GaP decomposition source. A 3 μm thick InGaP epilayer shows that low temperature photoluminescence (PL) peak energy is as large as 1.998 eV, full width at half maximum (FWHM) is 5.26 meV, which is the smallest ever reported, and X-ray diffraction (XRD) rocking curve linewidth is as narrow as that of GaAs substrate. The electron mobilities at room temperature of nominally undoped InGaP layers obtained by Hall measurements are comparable to similar InGaP epilayer grown by solid-source molecular beam epitaxy (SSMBE) with other sources or other growth techniques. The large area InGaP/GaAs HBTs show very good Dc characteristics.     

GaAs/AlGaAs异质结的界面束缚二维激子效应

本文讨论了GaAs/AlGaAs异质结界面的H线发光及其性能。用双晶X射线衍射及皮秒光致发光证明了H线与界面质量密切相关,并且有相似于激子跃迁的寿命行为。用限制于异质结界面势阱的二维电子(或空穴)与分布于GaAs边的三维空穴(或电子)组成的二维激子效应,解释了H线的实验结果。并讨论了不同外延生长的异质结与界面有关的发光行为。     

应变弛豫InGaAs/GaAs超晶格的X射线双晶衍射及形貌研究

应用X射线双晶衍射及双晶形貌术,对应变弛豫的InGaAs/GaAs超晶格作了研究,通过对双晶衍射摇摆曲线的计算机模拟,得到了超晶格的结构,应变弛豫机制,弛豫比,超晶格层与衬底的取向差等重要参数。从双晶形貌,得到了超晶格与衬底界面处和超晶格中的位错分布。 关键词：     

GaAs/Ge的MOCVD生长研究

用常压MOCVD在Ge衬底上外延生长了GaAs单晶层,研究了GaAs和6e的极性与非极性材料异质外延生长,获得了质量优良的GaAs/Ge外延片,GaAs外延层X射线双晶衍射回摆曲线半高宽达16弧秒.10K下PL谱半峰宽为7meV.讨论了极性与非极性外延的界面反相畴问题和GaAs-Ge界面的Ga、Ge原子互扩散问题.     

Be掺杂对InGaAsN/GaAs量子阱性能的提高

InGaAsN/GaAs量子阱中进行铍(Be)元素重掺杂能显著提高其光学性质,并且发光波长发生了红移.X射线衍射摇摆曲线清楚地证实了铍掺杂抑制了InGaAsN(Be)/GaAs量子阱在退火过程中的应力释放.对比退火前,退火后的没有进行铍掺杂的量子阱样品的量子阱的X射线摇摆曲线衍射峰明显向GaAs衬底峰偏移;而对于掺铍的量子阱样品而言,这样的偏移要小很多.     

Properties of a large La1.92Sr0.08CuO4+δ single crystal grown by the travelling-solvent floating-zone method

A centimeter size single crystal of La_2−xSr_xCuO_4+δ (volume=1.32 cm³) with x_Sr=0.08 has been grown by the travelling-solvent floating-zone (TSFZ) method using a double ellipsoidal-type optical furnace as the heat source. The crystallised phase was checked solvent free by X-ray powder diffraction experiments, the crystal dimensions and quality being investigated by X-ray and neutron Laüe techniques. Several rocking curves of the Bragg peaks were performed by neutron diffraction giving a full width at half maximum (FWHM) of 0.200° for (006) reflection and clearly showing the presence of twin domains as expected for such an orthorhombic structure. The superconducting critical temperature of the as-grown crystal under 2 oxygen bar was determined by SQUID measurements with T_c=18–20 K. Thermal treatments at different oxygen pressures were carried out showing no significant improvement of the transition sharpness and the T_c value. Normal state susceptibility was also measured from 6 to 800 K for two different field orientations and can be interpreted as an antiferromagnetic insulating state behaviour. The resistivity measurements display an insulating behaviour perpendicular to the CuO₂ planes and a metallic behaviour in the planes, with a high anisotropy ratio R_c/R_b350 at room temperature and a zero resistivity achieved at 27 K in both directions. The specific heat measurements have revealed no anomalies in the temperature range 15–300 K.     

Growth and characterization of rocksalt MnS/GaAs epilayers by hot-wall epitaxy

Epitaxial growth characteristics of α-MnS on GaAs(1 0 0) substrates have been investigated by X-ray diffraction and double crystal rocking curve measurements. Growth of stoichiometric α-MnS films has been performed by hot-wall epitaxy using Mn and ZnS as a source of sulfur. The films on GaAs(1 0 0) at low substrate temperature exhibit multiphase crystal structures of zincblende and rocksalt, and the main structure is changed to rocksalt with increasing substrate temperature. Photoluminescence spectrum of the α-MnS epilayer at 5 K exhibits broad emission bands, which are attributed to Mn²⁺ ions. The band gap energy of the α-MnS epilayer at room temperature was also estimated to be about 3.3 eV by reflection.     

The influence of SixNy interlayer on GaN film grown on Si(111) substrate

A method to drastically reduce dislocation density in a GaN film grown on an Si(111) substrate is newly developed. In this method, the Si_xN_y interlayer which is deposited on an AlN buffer layer in situ is introduced to grow the GaN film laterally. The crack-free GaN film with thickness over 1.7 micron is grown on an Si(111) substrate successfully. Synthesized GaN epilayer is characterized by X-ray diffraction (XRD), atomic force microscope (AFM), and Raman spectrum. The test results show that the GaN crystal reveals a wurtzite structure with the <0001> crystal orientation and the full width at half maximum of the X-ray diffraction curve in the (0002) plane is as low as 403 arcsec for the GaN film grown on the Si substrate with an Si_xN_y interlayer. In addition, Raman scattering is used to study the stress in the sample. The results indicate that the Si_xN_y interlayer can more effectively accommodate the strain energy. So the dislocation density can be reduced drastically, and the crystal quality of GaN film can be greatly improved by introducing Si_xN_y interlayer.     

垂直腔面发射激光器的结构生长及特性研究

在偏〈111〉A 2°的GaAs (100) 衬底上生长了Al0.9Ga0.1As /Al0.2Ga0.8As周期结构的垂直腔面发射激光器（VCSEL）外延片P 型DBR的周期数为24.5对,N型DBR的周期数为34.5对.用光荧光 (PL) 谱、扫描电子显微镜 (SEM)和X射线双晶衍射 (XRD) 方法对VCSEL的光学特性和结构特性进行了分析室温量子阱材料的PL谱峰值波长为837.0 nm,半高宽达到28.9 nm在X射线双晶衍射回摆曲线中,除了“0”级衍射峰外,还观察到一级和二级卫星峰.“0”级双晶衍射峰的半高宽为12.56弧秒(″),衬底GaAs的衍射峰半高宽为11.79″.“0”级衍射峰半高宽与衬底GaAs的衍射峰半高宽比较接近,表明晶格具有很高的完整性.实验结果表明腔模波长为837.2 nm,腔模波长与PL谱峰值波长相匹配.     

Structural and compositional analysis of InBixAsySb(1−x−y) films grown on GaAs(0 0 1) substrates by liquid phase epitaxy

The growth of epitaxial InBi_xAs_ySb_(1−x−y) layers on highly lattice mis-matched semi-insulating GaAs substrates has been successfully achieved via the traditional liquid phase epitaxy. Orientation and single crystalline nature of the film have been confirmed by X-ray diffraction. Scanning electron micrograph shows abrupt interface at micrometer resolution. Surface composition of Bi(x) and As(y) in the InBi_xAs_ySb_(1−x−y) film was measured using energy dispersive X-ray analysis and found to be 2.5 and 10.5 at.%, respectively, and was further confirmed with X-ray photoelectron spectroscopy. Variation of the composition with depth of the film was studied by removing the layers with low current (20 μA) Ar⁺ etching. It was observed that with successive Ar⁺ etching, In/Sb ratio remained the same, while the As/Sb and Bi/Sb ratios changed slightly with etching time. However after about 5 min etching the As/Sb and Bi/Sb ratios reached constant values. The room temperature band gap of InBi_0.025As_0.105Sb_0.870 was found to be in the range of 0.113–0.120 eV. The measured values of mobility and carrier density at room temperature are 3.1×10⁴ cm² V⁻¹ s⁻¹ and 8.07×10¹⁶ cm⁻³, respectively.     

Characterization of alloy composition in Ga1-xAlxAs/GaAs structures: comparison of photovoltage, X-ray, SIMS and RHEED techniques

A comparative study of techniques for the characterization of alloy composition in Ga_1-xAl_xAs/GaAs single and multilayer structures has been carried out. Good agreement (x ± 0.015) is demonstrated between double-crystal X-ray diffraction and photovoltage spectroscopy measurements using the generally accepted calibration of Casey and Panish. A slightly modified form of the band gap versus composition curve is presented which further improves the agreement to x±0.005. Profiling conditions achieving linear SIMS Al profiles are reported, yielding compositions in agreement with PVS and X-ray within x+-0.01 (when calibrated at a single composition). A systematic discrepancy between results from the above techniques and in-situ RHEED oscillation measurements is reported.     

多铁材料Bi1-xCaxFeO3的介电、铁磁特性和高温磁相变

采用溶胶凝胶法制备Bi_1-xCa_xFeO₃ (x=0, 0.05, 0.1, 0.15, 0.2)陶瓷样品. X衍射图谱表明所有样品的主衍射峰均与纯相BiFeO₃相符合且具有良好的晶体结构. 随着x的增大, Bi_1-xCa_xFeO₃样品的主衍射峰由双峰(104)与(110) 逐渐重叠为单峰(110), 当x ≥0.15时, 样品呈现正方晶系结构; 扫描电镜形貌分析可知, 晶粒由原来的0.5 μm逐渐增大到2 μm. Bi_1-xCa_xFeO₃样品介电常数和介电损耗随着x 的增加先增大而后减小. 当f=1 kHz, Bi_0.9Ca_0.1FeO₃ 的介电常数达到最大值, 是BiFeO₃的7.5倍, 而Bi_0.8Ca_0.2FeO₃的介电常数达到最小值, 仅仅是BiFeO₃的十分之一. Bi_1-xCa_xFeO₃样品所呈现的介电特性是由偶极子取向极化和空间电荷限制电流两种极化机理共同作用的结果. 随着Ca²⁺ 的引入, BiFeO₃ 样品的铁磁性显著提高. X射线光电子能谱图表明Fe²⁺和Fe³⁺ 共存于Bi_1-xCa_xFeO₃ 样品中, Fe²⁺/Fe³⁺比例随着Ca²⁺ 掺杂量的增加而增大, 证明Ca²⁺掺杂增加了Fe²⁺的含量, 增强BiFeO₃的铁磁特性. 从M-T曲线观察到BiFeO₃样品在878 K附近发生铁磁相变, 示差扫描量热法测试再次证明BiFeO₃ 在878 K发生相变. Ca²⁺掺杂使BiFeO₃样品的T_N略有变化而T_M基本不变, 其主要原因是Fe-O-Fe反铁磁超交换作用的强弱和磁结构相对稳定.     

Evaluation of threading dislocation density of strained Ge epitaxial layer by high resolution x-ray diffraction

The analysis of threading dislocation density(TDD)in Ge-on-Si layer is critical for developing lasers,light emitting diodes(LEDs),photodetectors(PDs),modulators,waveguides,metal oxide semiconductor field effect transistors(MOS-FETs),and also the integration of Si-based monolithic photonics.The TDD of Ge epitaxial layer is analyzed by etching or transmission electron microscope(TEM).However,high-resolution x-ray diffraction(HR-XRD)rocking curve provides an optional method to analyze the TDD in Ge layer.The theory model of TDD measurement from rocking curves was first used in zinc-blende semiconductors.In this paper,this method is extended to the case of strained Ge-on-Si layers.The HR-XRD 2θ/ωscan is measured and Ge(004)single crystal rocking curve is utilized to calculate the TDD in strained Ge epitaxial layer.The rocking curve full width at half maximum(FWHM)broadening by incident beam divergence of the instrument,crystal size,and curvature of the crystal specimen is subtracted.The TDDs of samples A and B are calculated to be 1.41×10~8cm~(-2)and 6.47×10~8cm~(-2),respectively.In addition,we believe the TDDs calculated by this method to be the averaged dislocation density in the Ge epitaxial layer.     

Strain due to nickel diffusion into hydrogen-terminated Si(1 1 1) surface

We studied the affection of thin (i.e., 0.2–0.8 nm) Ni films on hydrogen-terminated Si(1 1 1) substrate surface by using strain-sensitive X-ray diffraction. It was reported that Ni deposition onto hydrogen-terminated Si surface apparently does not cause film growth, but rather diffuses into the Si crystal, creating an “Ni diffusion layer” up to Ni deposition 0.8 nm thick. Measured rocking curves of the Si 1 1 3 reflection and integrated intensities of the rocking curves for the substrate provide information about the evolution of the strain field introduced near the substrate surface during Ni diffusion into the substrate. Comparing the measured and calculated rocking curves indicates that compression of the {1 1 1} spacing of the Si occurs gradually up to an Ni thickness of 0.6 nm, and that above this thickness, strain relaxation occurs.

We found that the slope of the integrated intensity of the rocking curve versus X-ray wavelength correlates to the strain field near the surface, in the same way that the shape of the rocking curves correlate to the strain field near the surface. Dynamical diffraction calculations indicate that measurement of the slope of the integrated intensity of the rocking curve versus X-ray wavelength is useful for strain analysis, because the dependence is not only sensitive to strain fields, but is also insensitive to the effect of absorption by the overlayer, which otherwise would cause deformation of the shape of the rocking curve.     

Preparation and structural properties of MgO films grown on GaAs substrate

Epitaxial MgO thin films have been grown on semiinsulating GaAs (0 0 1) substrates using electron beam (e-beam) evaporation. X-ray diffraction indicates c-axis oriented MgO with (0 0 2) reflection only and rocking curve widths ∼2.2-3°. Transmission electron microscopy (TEM) analyses confirm an epitaxial growth of the MgO films. We study the microstructure and the defects at the interface between the MgO film and the GaAs substrate. Auger electron Spectroscopy (AES) concentration depth profiles reveal no contamination of the MgO films by As and Ga at different temperatures of the deposition process.     

New experimental evidence of the structural modification in single crystal Bi2Sr2CaCu2Oy by X-ray diffraction observation

The variations of the high angle 00 peak-shape by means of X-ray l scans of the 00l fundamental reflections were investigated in detail for a highly oriented Bi₂Sr₂CaCu₂O_y (Bi2212) crystal with sufficiently small intrinsic mosaicity and the same crystal annealed in air at 250, 300, 400, 600, and 750°C for 20 h in consequence. For the first time, we observed a new additional reflection almost overlapped original 00l fundamental reflection at annealing temperature below 400°C by X-ray diffraction measurement, which shows that there coexisted two sets of lattice periodicity in the c-direction of the annealed crystal. The new additional reflection appeared at 250°C and disappeared at 400°C. Its intensity was increased at 300°C. The measurements of the AC susceptibility, c-axis parameter and full width at half maximum (FWHM) of the 00 peaks showed that the new additional reflection was associated with the oxygen diffusion in CuO₂ planes and the changes of strain field. The results provide the new experimental evidence that the structural distortion is more sensitive to the oxygen diffusion in CuO₂ planes than to that in Bi–O layers.     

GaSb/AlSb/GaAs应变层结构的分子束外延生长

本文以反射式高能电子衍射(RHEED)和其强度振荡为监测手段,在半绝缘GaAs衬底上成功地生长GaSb/AlSb/GaAs应变层结构,RHEED图样表明,GaSb正常生长时为Sb稳定的C(2×6)结构,AlSb为稳定的(1×3)结构,作者观察并记录GaSb,AlSb生长时的RHEED强度振荡,并利用它成功地生长10个周期的GaSb/AlSb超晶格,透射电子显微镜照片显示界面平整、清晰,采用较厚的AlSb过渡层及适当的生长条件,可在半绝缘GaAs衬底上生长出质量好的GaSb外延层,其X射线双晶衍射半峰宽小于 关键词：     

高完整GexSi1-x/Si应变超晶格的X射线双晶衍射研究

本文用X射线双晶衍射技术对分子束外延生长的Ge_xSi_1-x/Si应变超晶格的结构参数进行研究,分别采用X射线运动学理论和动力学理论对超晶格的双晶摆动曲线进行计算模拟,得出超晶格的全部结构参数;并对这两种理论计算模拟的结果进行比较,发现这两种理论计算的结果基本一致,只是在细微结构上略有差别,对高完整Ge_xSi_1-x/Si超晶格,用动力学理论计算的曲线更接近于实验曲线。 关键词：     

Dislocation distributions and tilts in Al(Ga)InAs reverse-graded layers grown on misorientated GaAs substrates

Compositionally undulating step-graded Al(Ga)In_xAs(x = 0.05–0.52) buffers with the following In P layer were grown by metal–organic chemical vapor deposition(MOCVD) on(001) GaAs with a 15°miscut. The dislocation distribution and tilts of the epilayers were examined using x-ray rocking curve and(004) reciprocal space maps(RSM) along two orthogonal 《110》 directions. The results suggested that such reverse-graded layers have different effects on α and βdislocations. A higher dislocation density was observed along the [110] direction and an epilayer tilt of-1.43°was attained in the [1-10] direction when a reverse-graded layer strategy was employed. However, for conventional step-graded samples,the dislocation density is normally higher along the [1-10] direction.