GaP?AlxGa1−xP heterostructure edge coupling waveguides for hybrid integrated optic devices

In this paper we present the performance of GaP Al_xGa_1−xP heterostructure waveguides for integrated optic hybrid devices. The waveguide layer is graded with a parabolic refractive index profile for the light emission of a DH GaAs semiconductor laser. The waveguide heterostructure performed allows to couple at it edge crossection semiconductor laser or photodetector as well as fix or solder them on the same substrate on which the heterostructure layers were deposited. The heterostructure layers were grown by liquid phase epitaxy and the heterostructure waveguide was performed by means of etching technics specially developed for this purpose. Both, the growth procedure, as well as the etching technics are described. The results achieved are shown in curves and photographs, taken on a scanning microscope.     

Ti3C2Tx MXene制备及在超级电容器中的应用研究进展

二维材料(2D)MXenes因其具有高比表面积、高导电率、可溶液加工等特性,作为超级电容器电极材料受到广泛关注。本文中总结了基于HF和氟化盐的刻蚀、基于碱的刻蚀、电化学刻蚀、路易斯酸熔融盐刻蚀等几种Ti₃C₂T_x MXene的制备方法,综述了真空辅助过滤、阳离子自组装、逐层组装工艺、印刷工艺、组装MXene气凝胶和水凝胶等Ti₃C₂T_xMXene基电极材料的组装策略及其在超级电容器的应用。研究表明,不同制备方法和电极组装策略将会影响电极材料的结构和电化学性能。对Ti₃C₂T_x MXene的制备方法和电极组装策略进行了对比总结,指出了研究中存在的问题,并展望了MXene今后的研究方向。     

Wet KOH etching of freestanding AlN single crystals

We investigated defect-selective wet chemical etching of freestanding aluminum nitride (AlN) single crystals and polished cuts in a molten NaOH–KOH eutectic at temperatures ranging from 240 to 400 °C. Due to the strong anisotropy of the AlN wurtzite structure, different AlN faces get etched at very different etching rates. On as-grown rhombohedral and prismatic facets, defect-related etching features could not be traced, as etching these facets was found to mainly emphasize features present already on the un-etched surface. On nitrogen polar basal planes, hexagonal pyramids/hillocks exceeding 100 μm in diameter may form within seconds of etching at 240 °C. They sometimes are arranged in lines and clusters, thus we attribute them to defects on the surface, presumably originating in the bulk material. On aluminum polar basal planes, the etch pit density which saturates after approx. 2–3 min of total etching time at 350 °C equals the density of a certain type of dislocations (presumably screw dislocations) threading the surface. Smaller etch pits form around annealed indentations, in the vicinity of some bigger etch pits after repeated etching, and sometimes also isolated on the surface area. Although alternate explanations exist, we attribute these etch pits to threading mixed and edge dislocations. This paper features etching parameters optimized for different planes and models on the formation of etching features especially on the polar faces. Finally, the issue of reliability and reproducibility of defect detection and evaluation by wet chemical etching is addressed.     

Growth and morphology of the CuGaS2, CuAlSe2, CuGaSe2 and CuInS2 ternary compounds

Monocrystals of the ternary compounds CuGaS₂, CuAlSe₂, CuGaSe₂, and CuInS₂ were grown from their elements by transport reactions; their cell parameters and melting temperature were determined. The character of the phase transition in these compounds was found out and also the boundary conditions of growing the monocrystals as well as their dislocation structure (by etching).     

Development of chalcogenide glass photoresists for gray scale lithography

Wet and dry negative etching procedures are evaluated for the fabrication of 3D graded microstructures in As–S based inorganic photoresists. Absorption of light and consequent photostructural changes near the surface layer enhance the chemical resistance of the As–S films. The success of the procedure is demonstrated by fabricating arrays of 12 μm diameter microlenses in a thin As₃₅S₆₅ film using a gray scale Cr mask and wet etching. The selectivity of dry etching is successfully realized by using photodiffusion in Ag–As₂S₃ bilayer structure. In this case, however, surface roughness or ‘grass’ is observed after etching. An unexpected segregation of silver is observed at the edges and at the boundary between the exposed and unexposed regions, which is investigated by SEM and XPS.     

CdS纳米棒的水热法制备及形成机理研究

采用水热法以Na2S· 9H2O为硫源,Cd3O12S3·8H2O为镉源,PVP为表面活性剂,成功制备了CdS纳米棒.并利用X射线衍射(XRD)、透射电子显微镜(TEM)和相应选区电子衍射(SAED)、高分辨透射电子显微镜(HRTEM)、X射线能量色散分析谱仪(XEDS)和紫外可见(UV-vis)分光光度计等测试手段对样品的晶体结构、形貌、微观结构和光学特性等特征进行了表征分析,实验结果表明本方法所制备的CdS纳米棒为纤锌矿结构,沿[001]方向择优生长,平均直径大约为50 nm,棒宽均匀、分散性好,带隙为2.43 eV.同时也对CdS纳米棒的形成机理进行了初步探讨,提出了CdS纳米棒的生长模型,其形貌从三角形到阶梯形棒晶,最后再到完整的棒状晶体的一个定向团聚的自组装过程.     

Plasma Etching of Niobium-SiOx Layers

CF₄-plasma etching of niobium and SiO_x layers has been investigated in a r.f. diode reactor. Etch rates increase linearly with increasing power density and also increase with pressure. The etch rate ratio can be changed using different etch gases or operating in different plasma modes (PE or IEPE). Changing from the ion enhanced plasma etching mode (IEPE) to plasma etching mode (PE) the etch rate ratio is changing by an factor of ten. On the basis of etch rate dependences on process parameters and thermodynamic data it has been suggested the generation of flourine radicals as the rate limiting step. A general etching model has been proposed, which explains qualitavelty and quantitatively (on account of data from literature) the measured results.     

Etching of Anthracene Cleavages in Sulphuric Acid — Formic Acid Solutions

Crystal etching, though a simple and widely adopted technique for the study of imperfections in a wide variety of materials, the process is not very well understood. The etch pit shapes are controlled by a number of factors, such as, the composition of etchant, the period of etching, the temperature of etching and the symmetry of plane under study. This communication reports observations of etching the (001) cleavage planes of anthracene in sulphuric acid — formic acid mixtures.     

Processing optimization and optical properties of 3-D photonic crystals

The synthesis optimization of three-dimensional photonic crystals (direct and inverse opals) is discussed in terms of the influence of processing parameters on the final optical quality. A colloidal/sol–gel route, starting with the self-organization of polystyrene microspheres into opal structures by convective self-assembly, followed by infiltration with a dielectric matrix precursor sol and heat treatment, has been followed. Several substrate hydrophilization methods have been tested and different substrates. Sol–gel infiltration of the opal template interstices with silica was achieved by dip-coating or micro-syringe application and it was followed by removal of the polymeric template. The concentration of the colloidal sol, containing polystyrene spheres of 235 or 460 nm in diameter, was optimized. The structural and optical properties of the opals and inverse opals have been studied by field emission scanning electron microscopy and optical reflectivity spectroscopy, in order to assess the relationship between their structure and the photonic properties obtained. By using borosilicate glass substrates hydrophilized with hydrochloric acid, colloidal photonic crystals of good quality have been obtained, with well ordered regions up to ～100 μm². By monitoring the effective refractive index change with relative humidity of the surrounding atmosphere, using spectroscopic ellipsometry with an environmental chamber, it was concluded that the present photonic crystals are suitable for humidity sensing applications.     

反应离子刻蚀制备石墨烯纳米盘阵列

采用化学气相沉积法以乙醇为碳源在铜箔生长的单层高质量的石墨烯并将其转移到SiO2/Si基底上。然后在通过自组装的方法在石墨烯表面覆盖一层单层的PS微球阵列。采用反应离子刻蚀的方法在一定的刻蚀条件下对其进行刻蚀,随着刻蚀的时间增加,PS微球的会被逐渐刻蚀掉,石墨烯也会在这个过程中随着被刻蚀。将残留的PS微球杂质去掉后,会在 SiO2/Si基底上呈现出排列规整的石墨烯纳米盘阵列。通过场发射扫描电子显微镜( SEM)、拉曼光谱对石墨烯纳米盘及其形成过程进行表征和分析,为后续制备高质量石墨烯纳米带、石墨烯纳米点、石墨烯纳米盘提供参考。     

Hydrothermal etching of flux grown phenakite (Be2SiO4) single crystals

The etching studies were made on flux grown phenakite (Be₂SiO₄) single crystals to elucidate the twinning phenomenon and the growth mechanism. The sharp and distinct etch pits and the twin boundaries were successfully obtained after the hydrothermal etching. From the etching and the X-ray precession experiments, it was conjectured that the phenakite had an inversion twin along the c axis. The twinning should be originated during the earlier stage of growth where the dendritic and acicular crystals were grown and thereafter the twinned crystals grew to the prismatic crystals during the latter stage with decreasing the temperature.     

Design and synthesis of large-pore p6mm mesoporus zirconia thin films templated by a novel block copolymer

A novel poly(butadiene-b-ethylene oxide) (PB-PEO) block copolymer was employed as the structure-directing agent for the preparation of large-pore, mesoporous for zirconia with two-dimensional (2D) hexagonal (p6mm) mesostructure through evaporation-induced self-assembly (EISA) approach. The presented materials, calcined at 400 °C and 500 °C, were characterized in detail by X-ray diffraction, transmission electron microscopy, and nitrogen sorption. The results showed that the mesoporous zirconia possesses a large-pore diameter, high BET surface area, and large-porosity. A probable formation mechanism was also presented in this work.     

Preparation of sapphire substrates for Gas phase GaN epitaxial processes

After mechanical treatment the surface of α-Al₂O₃ plates with orientation (0001) for GaN epitaxy was polished in a mixture of H₃PO₄ and H₂SO₄. The best mixture H₂SO₄/H₃PO₄ and the best temperature for polishing were chosen. — The quality of the polished substrates was determined by structural etching in KOH. The optimum structural etching time was 3 min. at 320°C. The thickness of the layer which should be removed after mechanical treatment and the dislocation density of the starting material for GaN epitaxy was determined.     

Studies on conventional and Sankaranarayanan–Ramasamy (SR) method grown ferroelectric glycine phosphite (GPI) single crystals

Transparent single crystals of glycine phosphite were grown by Sankaranarayanan–Ramasamy (SR) method and conventional slow evaporation solution technique (SEST) which had the sizes of 100 mm in length, 30 mm diameter and 10×11×8 mm³. The conventional slow evaporation and Sankaranarayanan–Ramasamy method grown glycine phosphite single crystals were characterized using laser damage threshold, chemical etching, Vickers microhardness, UV–vis–NIR and dielectric analysis. The laser damage threshold value was higher in SR method grown GPI crystal as against conventional method grown crystal. The SR method grown GPI has higher hardness and also higher transmittance compared to conventional method grown crystal. The chemical etching and dielectric loss measurements indicate that the crystal grown by SR method has low density of defects and low value of dielectric loss compared to conventional method grown GPI crystal.     

Determination of the Thickness of Chemically Removed Thin Layers on GaAs VPE Structures

Thinning of epitaxial GaAs layers was studied during the surface etching, with a special attention to submicron epitaxial structures, like MESFET or varactor-type structures. Each chemical treatment influences the crystal surface during the device preparation processes, though the possible thinning of the active layer is small. Therefore a method allowing determination of thicknesses as small as at about 20 nm of the layer removed by chemical etching from GaAs VPE structures was applied. Using special multilayered structures and a continuous electrochemical carrier concentration depth profiling, the influence of the layer thickness inhomogeneity and of some measurement errors can be minimized. Some frequently used etchants and the influence of different – so called – non-etching processes were compared in different combinations. It was shown that besides the direct etching a change of the surface conditions occurs, which influences the etch rate in the succeeding etching procedure.     

Unidirectional growth of l-asparagine monohydrate single crystal: First time observation of NLO nature and other studies of crystalline perfection,optical, mechanical and dielectric properties

L-asparagine monohydrate (LAM), a new amino acid single crystal, was grown by slow evaporation solution technique (SEST) as well as by recently invented Sankaranarayanan–Ramasamy (SR) method in aqueous medium. Using SR method, LAM single crystal of diameter ∼18 mm and length ∼52 mm was grown for the first time. The growth conditions were optimized and the maximum growth rate of 1.0 mm per day was observed for the SR crystal. The crystal structure was confirmed by powder XRD. The crystalline perfection was assessed by high resolution XRD and etching studies and found that the quality of the SR crystal is better than the SEST crystal. The UV–vis–NIR spectroscopic study revealed that the SR crystal has good optical transparency than that of SEST crystal. The relative second harmonic generation efficiency was measured and found to be ∼0.35 times to that of KDP. The laser damage threshold (LDT) was measured and found that the SR crystal has higher LDT value (5.76 GW cm⁻²) than SEST crystal (4.75 GW cm⁻²). The Vickers’s microhardness and dielectric studies were also carried out and discussed.     

Problems of Surface Morphology and Layer Deposition during Plasma Etching Processes (II) Si-etching in CF4-, CF4/O2-and CF4/H2 Plasmas

The plasma etching of Si in CF₄-, CF₄/O₂-and CF₄/H₂ plasmas was investigated in dependence on the etching gas, the plasma conditions (pressure, power density) and etching time in different reactors. A roughening of the surface and the formation of a “semi-amorphous” surface layer with a power-like morphology was detected by TEM-and RHEED methods. It is supposed that the surface layer has a fundamental consequence as an intermediate state in the etching mechanism.     

The K2S2O8–KOH photoetching system for GaN

A recently developed photoetching system for n-type GaN, a KOH solution containing the strong oxidizing agent potassium peroxydisulphate (K₂S₂O₈), was studied in detail. By careful selection of the etching parameters, such as the ratio of components and the hydrodynamics, two distinct modes were defined: defect-selective etching (denoted by KSO-D) and polishing (KSO-P). Both photoetching methods can be used under open-circuit (electroless) conditions. Well-defined dislocation-related etch whiskers are formed during KSO-D etching. All types of dislocations are revealed, and this was confirmed by cross-sectional TEM examination of the etched samples. Extended electrically active defects are also clearly revealed. The known relationship between etch rate and carrier concentration for photoetching of GaN in KOH solutions was confirmed for KSO-D etch using Raman measurements. It is shown that during KSO-P etching diffusion is the rate-limiting step, i.e. this etch is suitable for polishing of GaN. Some constraints of the KSO etching system for GaN are discussed and peculiar etch features, so far not understood, are described.     

绒毛球状碳酸锶的沉淀法制备与表征

以柠檬酸三钠为晶形控制剂,采用简单沉淀法合成了绒毛球状SrCO3晶体.用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶红外光谱仪(FTIR)、热重分析仪(TG)、透射电镜(TEM)和能谱仪(EDX)等对样品的结构和形貌进行了表征.结果表明,绒毛球状SrCO3的主体结构为微米级实心球,实心球壳表面被一层稠密的粒径为5～15 nm、长度为100 ～ 150 nm的毛发状晶体所覆盖;机理分析认为绒毛球状SrCO3的形成可以用“棒状-束状-哑铃形-球形”的生长机理(RBDS)进行解释.     

Dislocation studies by chemical etching on solution-grown NaSbF4 and Na3Sb4F15 single crystals

An attempt has been made to study the etch pit dislocations of isolated as well as matched pairs of cleavage planes of solution grown NaSbF₄ and Na₃Sb₄F₁₅ single crystals when etched with analar grade methyl alcohol and ethyl alcohol. On etching of cleavage faces the pits nucleate at the intersection sites of dislocations with the cleavage face. On successive etching of a cleavage face, arrays of triangular shape etch pits are observed. After prolonged etching some of the etch pits disappear. These pits are curved and terminated indicating that they are crystallographically non-oriented. One-to-one correspondence with respect to number, shape, position and structure of the pits has been established by etching of a matched cleavage face. The etch pit densities of both NaSbF₄ and Na₃Sb₄F₁₅ crystals are found to be 10³ per cm².