998 resultados para hydrothermal crystal growth


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采用中频感应提拉法生长了高质量的Tm:Y2SiO5(Tm:YSO)晶体,测定了晶体的晶格常数和分凝系数.运用劳厄照相法确定了单斜晶系Tm:YSO晶体的三个偏振轴〈010〉,D1和D2,在室温下测量了三个偏振轴方向的吸收光谱、荧光光谱和荧光寿命,计算了晶体吸收峰的吸收线宽和吸收截面.研究发现,相对于其他两个偏振轴方向,D1方向在790 nm处出现较强的吸收峰,同时在2μm附近出现了一定强度的发射峰,D1方向的吸收截面较大,荧光寿命较长.Tm:YSO晶体适用于AlGaAs二极管抽运固体激光器,在2μm波段固体激光器的应用上将有很大的发展潜力.

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Thin films of ZrO2, HfO2 and TiO2 were deposited on kinds of substrates by electron beam evaporation (EB), ion assisted deposition (IAD) and dual ion beam sputtering (DIBS). Then some of them were annealed at different temperatures. X-ray diffraction (XRD) was applied to determine the crystalline phase and the grain size of these films, and the results revealed that their microstructures strongly depended on the deposition conditions such as substrate, deposition temperature, deposition method and annealing temperature. Theory of crystal growth and migratory diffusion were applied to explain the difference of crystalline structures between these thin films deposited and treated under various conditions. (c) 2007 Elsevier B.V. All rights reserved.

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一,缺失nifZ的棕色固氮菌突变种钼铁蛋白的晶体生长的研究进展 在一定的结晶条件下,缺失nifZ的棕色固氮菌突变种钼铁蛋白将从溶液中结晶出深棕色的短斜四棱柱晶体。PEG 8000、MgCl2、NaCl、Tris的浓度及缓冲液的pH对该蛋白的结晶及晶体生长影响的系统研究表明,它们的浓度和pH较低时,不出晶体;当pH高于8.0,随着前三种化合物浓度的逐渐提高,便在一周内出现大量小品体;再提高浓度后,便延长结晶时问但出质好、数少而个大的晶体;然后晶体随浓度的提高而又变小、变多、甚至晶质变差,直至不再出晶体。影响晶体生长的各因子的最适浓度随其它条件的改变而有所不同。当缓冲液的pH为8.2而PEG 8000,MgCl’、NaCI、蛋白质和Tris的浓度分别为1.86%、300 mmol/L、400 mmoUL、4.64g/L、53 mmo/L时,首次发现在一滴悬滴结晶液中只有一颗较大的优质晶体(最大两边线度均为0.16mm)。 二,从分别含Mn和Cr的培养基中生长的固氮菌突变种UW3中纯化的固氮酶的特性和结晶 缺失nifH基因的棕色固氮菌突变种UW3,在有钼环境中不能固氮生长,但能在无钼而含MnS01或Na2Cr01的无氮培养基中固氮生长。分别经超声破碎、加热除去部分杂蛋白、离子交换柱层析和Sephacryl S-200或S-300柱层析的分离纯化,分别得到二种固氮酶组分l蛋白。金属元素测定表明,这两种蛋白除含铁元素外还分别含有锰和铬元素。它们的吸收光谱、CD和AR谱互不完全相同,并都与OP-MoFe蛋白存在较大差异。含Mn固氮酶也能还原C2H2、质子和N2,对它们的还原的比活性都分别约为MoFe蛋白活性的50%。初步结果表明,这一突变种在这两种培养条件下都可能已表达了不同于已发现的三种固氮酶的新固氮酶组分l蛋白-MoFe、VFe和FeFe蛋白,分别为含Mn或Cr的固氮酶组分1蛋白,分别被称为uw3,-MnFe蛋白和UW3-CrFe蛋白。通过对PEG 8000、MgCI2、NaCI和缓冲液的种类和浓度等结晶条件的大量优化组合实验,首次获得uw3-MnFe蛋白和UW3-CrFe蛋白的的晶体。最大晶体为21.4×14.3×2.1μm。

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一、棕色固氮菌突变种DJ35固氮酶钼铁蛋白的纯化、体外重组及结晶研究   棕色固氮菌(Azotobacter vinelandii Lipmann)突变种DJ35的菌体破碎后,所得的未经加热的粗提物经DEAE Cellulose 52柱层析后得到部分纯的钼铁蛋白(ΔnifE Av1)和铁蛋白(Av2)。部分纯的ΔnifE Av1再经Sephacryl S-300和Q-Sepharose Fast Flow柱层析进一步纯化,便首次得到SDS凝胶电泳检测为基本纯的ΔnifE Av1。SDS-PAGE及Western blotting的结果表明,ΔnifE Av1具有与野生型棕色固氮菌钼铁蛋白(OP Av1)相同的亚基种类和组成(α2β2)。质子还原活性测定表明,在与Av2进行活性互补时ΔnifE Av1不具有明显的质子还原活性,而与从OP Av1抽提出的FeMoco抽提液保温后便可与Av2实现活性互补。这表明,ΔnifE Av1是一种缺失FeMoco的钼铁蛋白。   将ΔnifE Av1用过量的邻菲啰啉(o-phenanthroline)厌氧处理并经Sephadex G-25柱层析分离后,便得到部分丢失Fe的ΔnifE Av1©。在同时存在Av2和MgATP发生系统的条件下,ΔnifE Av1©, 而不是处理前的ΔnifE Av1,可为由KMnO4或Na2CrO4、高柠檬酸铁、Na2S、Na2S2O4 和二硫苏糖醇组成的含Mn或含Cr重组液(RS-Mn或RS-Cr)显著激活,但在缺少MgATP或Av2的条件下,RS-Mn和RS-Cr则不能激活ΔnifE Av1©。这就表明,RS-Mn和RS-Cr对ΔnifE Av1©的激活都需要邻菲啰啉的预处理及Av2和MgATP的同时存在。从分别缺失nifZ和nifB点突变的固氮菌突变种DJ194和UW45中纯化得到的钼铁蛋白,ΔnifZ Av1和NifB- Av1,经邻菲啰啉厌氧处理并经Sephadex G-25柱层析分离后,也分别得到部分丢失Fe的ΔnifZ Av1©和NifB- Av1©。与ΔnifE Av1©一样,这两种蛋白在Av2和MgATP同时存在时也可被RS-Cr和含Mo重组液(RS-Mo)明显激活。   为获得可供X-射线衍射的ΔnifE Av1的大单晶,对组成蛋白质沉淀剂的各种化合物的种类和浓度、缓冲液的pH值、结晶方法及蛋白样品的批次、浓度等结晶条件进行了大量优化研究。首次获得了ΔnifE Av1的深棕色短斜四棱柱晶体,并对其蛋白组成进行了鉴定。 二、铬铁蛋白中残存的棕色固氮菌细菌铁蛋白的晶体生长及鉴定   从无钼、无氨而含铬的固氮培养基中生长的棕色固氮菌突变种UW3中纯化得到了部分纯的CrFe蛋白。在试图培养CrFe蛋白大晶体时发现,棕色晶体和砖红色晶体可同时或单独出现。SDS-和厌氧天然-PAGE皆表明,棕色晶体主要由与Av1类似大小的亚基(~60 kD)组成,而砖红色晶体则主要由~20 kD亚基组成。Western-blotting表明只有~60 kD亚基可与OP Av1的抗体发生反应,而~20 kD亚基则无这种反应。在部分纯的CrFe蛋白中,~20 kD的蛋白含量远低于~60 kD蛋白的含量,表明由这种小亚基组成的蛋白只是CrFe蛋白中的一种污染蛋白。用3,5-二氨基苯甲酸染色的天然电泳表明,形成砖红色和棕色晶体的蛋白是迁移率不同的两种含铁蛋白。质谱分析表明,该晶体蛋白为棕色固氮菌的细菌铁蛋白(AvBF)。分辨率为2.34 Å的X-射线衍射结果也表明,砖红色晶体属于H3空间群,晶胞参数为a = 124.965 Å, b= 124.965 Å 和 c = 287.406 Å。首次完成的结构解析也表明,这种砖红色晶体确为24聚体的AvBF。 关键词:棕色固氮菌突变种DJ35和UW3; ΔnifE Av1; 铬铁蛋白; 细菌铁蛋白; 纯化和特性; 体外激活组装; 晶体生长及组成鉴定

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我们从A. vinelandii突变株DJ35中纯化得到了ΔnifE Av1,并通过与OP Av1相比较对其特性进行了研究。虽然ΔnifE Av1以四聚体形式(α2β2)存在,但却表现出两种天然电泳行为。与OP Av1相比,ΔnifE Av1中的金属含量较低,每个蛋白分子仅含9.96个铁原子、0.36个钼原子。OP Av1和ΔnifE Av1的吸收光谱相似,均在280 nm附近出现蛋白吸收峰,在300-600 nm波长范围内光吸收普遍降低,并无特征峰出现。虽然ΔnifE Av1可见光区域CD谱的摩尔消光系数(Δε)总比OP Av1小,但在520nm区域附近摩尔消光系数减少的相对值明显大于在450nm附近摩尔消光系数减少的相对值。ΔnifE Av1的EPR信号明显与OP Av1不同,在g≈3.7处的EPR信号完全消失,在g≈4.3 和2.0处的EPR信号强度也分别降低了75%和50%以上。ΔnifE Av1不能与Fe蛋白组成活性单位,但被FeMoco激活后可与Fe蛋白组成活性单位。上述结果表明, ΔnifE Av1不含FeMoco,但具有与OP Av1相同的P-cluster。 我们在纯化ΔnifE Av1的过程中,发现一个类似OP Av1的β亚基的污染蛋白,经MALDI-TOF质谱鉴定这种蛋白是棕色固氮菌中一预测基因的产物。通过改进纯化方法, 我们首次得到80%电泳纯的蛋白,并将其命名为HBP59蛋白。HBP59为一单体蛋白,分子量约为59k Da。金属测定结果表明每个蛋白分子中含有0.42个铁原子。HBP59蛋白的可见光谱表现出典型的血红素蛋白光谱特征,还原态的HBP59蛋白在421nm处有最大吸收峰,同时在517nm、556nm处有两个伴随肩峰出现, A421/A280仅为0.146。HBP59蛋白氧化后,吸收峰发生蓝移,最大吸收峰从421nm移到413nm,517nm和556nm处的肩峰消失,A413/A280为0.168。HBP59蛋白的可见光区圆二色谱比较复杂,正峰出现在420nm, 406nm, 379nm 和364nm; 其摩尔消光系数分别为0.75, 0.94, 0.68 和 0.99;负峰出现在433 nm 和392nm,其摩尔消光系数分别为-1.13 和-0.78。血红素滴定实验结果说明每个HBP59蛋白分子结合了0.1个血红素,但每个蛋白分子具有最大结合1个血红素的能力。这低结合能力与这低比率的比率是非常一致的。该蛋白对温度相对敏感,高于40℃蛋白开始沉淀。上述结果说明HBP59是一个结合具有低自旋和不对称的血红素的蛋白,它在菌体内可能并未扮演贮藏血红素的角色,而是可能参与血红素的运输或附着。 此外,经过结晶条件的大量筛选后获得了ΔnifE Av1和ΔnifH Av1的优质小单晶,并对HBP59的晶体培养进行了初步探索。

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Hybrid nanostructured materials can exhibit different properties than their constituent components, and can enable decoupled engineering of energy conversion and transport functions. Novel means of building hybrid assemblies of crystalline C 60 and carbon nanotubes (CNTs) are presented, wherein aligned CNT films direct the crystallization and orientation of C 60 rods from solution. In these hybrid films, the C 60 rods are oriented parallel to the direction of the CNTs throughout the thickness of the film. High-resolution imaging shows that the crystals incorporate CNTs during growth, yet grazing-incidence X-ray diffraction (GIXD) shows that the crystal structure of the C 60 rods is not perturbed by the CNTs. Growth kinetics of the C 60 rods are enhanced 8-fold on CNTs compared to bare Si, emphasizing the importance of the aligned, porous morphology of the CNT films as well as the selective surface interactions between C 60 and CNTs. Finally, it is shown how hybrid C 60-CNT films can be integrated electrically and employed as UV detectors with a high photoconductive gain and a responsivity of 10 5 A W -1 at low biases (± 0.5 V). The finding that CNTs can induce rapid, directional crystallization of molecules from solution may have broader implications to the science and applications of crystal growth, such as for inorganic nanocrystals, proteins, and synthetic polymers. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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Taper-free and vertically oriented Ge nanowires were grown on Si (111) substrates by chemical vapor deposition with Au nanoparticle catalysts. To achieve vertical nanowire growth on the highly lattice mismatched Si substrate, a thin Ge buffer layer was first deposited, and to achieve taper-free nanowire growth, a two-temperature process was employed. The two-temperature process consisted of a brief initial base growth step at high temperature followed by prolonged growth at lower temperature. Taper-free and defect-free Ge nanowires grew successfully even at 270 °C, which is 90 °C lower than the bulk eutectic temperature. The yield of vertical and taper-free nanowires is over 90%, comparable to that of vertical but tapered nanowires grown by the conventional one-temperature process. This method is of practical importance and can be reliably used to develop novel nanowire-based devices on relatively cheap Si substrates. Additionally, we observed that the activation energy of Ge nanowire growth by the two-temperature process is dependent on Au nanoparticle size. The low activation energy (∼5 kcal/mol) for 30 and 50 nm diameter Au nanoparticles suggests that the decomposition of gaseous species on the catalytic Au surface is a rate-limiting step. A higher activation energy (∼14 kcal/mol) was determined for 100 nm diameter Au nanoparticles which suggests that larger Au nanoparticles are partially solidified and that growth kinetics become the rate-limiting step. © 2011 American Chemical Society.

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We report straight and vertically aligned defect-free GaAs nanowires grown on Si(111) substrates by metal-organic chemical vapor deposition. By deposition of thin GaAs buffer layers on Si substrates, these nanowires could be grown on the buffer layers with much less stringent conditions as otherwise imposed by epitaxy of III-V compounds on Si. Also, crystal-defect-free GaAs nanowires were grown by using either a two-temperature growth mode consisting of a short initial nucleation step under higher temperature followed by subsequent growth under lower temperature or a rapid growth rate mode with high source flow rate. These two growth modes not only eliminated planar crystallographic defects but also significantly reduced tapering. Core-shell GaAs-AlGaAs nanowires grown by the two-temperature growth mode showed improved optical properties with strong photoluminescence and long carrier life times. © 2011 American Chemical Society.

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The influence of well thickness on the electroluminescence (EL) of InGaN/GaN multiple quantum wells (MQWs) grown by metalorganic chemical vapor deposition is investigated. It is found that the peak wavelength of EL increases with the increase of well thickness when the latter is located in the range of 3.0-5.1 nm. The redshift is mainly attributed to the quantum confined Stark effect (QCSE). As a contrast, it is found that the EL intensity of InGaN/GaN MQWs increases with the increase of well thickness in spite of QCSE. The result of X-ray diffraction demonstrates that the interface become smoother with the increase of well thickness and suggests that the reduced interface roughness can be an important factor leading to the increase of EL intensity of InGaN/GaN MQWs. (C) 2009 Elsevier B.V. All rights reserved.

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In this paper, we obtain SiGe quantum dots with the diameters and density of 15-20 nm and 1.8 x 10(11) cm(-2), respectively, by 193 nm excimer laser annealing of Si0.77Ge0.23 strained films. Under the excimer laser annealing, only surface atoms diffusion happens. From the detailed statistical information about the size and shape of the quantum dots with different annealing time, it is shown that the as-grown self-assembled quantum dots, especially the {105}-faceted dots, are not stable and disappear before the appearance of the laser-induced quantum dots. Based on the calculation of surface energy and surface chemical potential, we show that the {103}-faceted as-grown self-assembled quantum dots are more heavily strained than the {105}-faceted ones, and the heavy strain in the dot can decrease the surface energy of the dot facets. The formation of the laser-induced quantum dots, which is also with heavy strain, is attributed to kinetic constraint. (c) 2008 Elsevier B.V. All rights reserved.

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AlGaInP/GaInP quantum well intermixing phenomena induced by Zn impurity diffusion at 540 degrees C were studied using room-temperature photo luminescence (PL) spectroscopy. As the diffusion time increased from 40 to 120 min, PL blue shift taken on the AlGaInP/GaInP quantum well regions increased from 36.3 to 171.6 meV. Moreover, when the diffusion time was equal to or above 60 min, it was observed firstly that a PL red shift occurred with a PL blue shift on the samples. After detailed analysis, it was found that the red-shift PL spectra were measured on the Ga0.51In0.49P buffer layer of the samples, and the mechanism of the PL red shift and the PL blue shift were studied qualitatively. (C) 2007 Elsevier B.V. All rights reserved.

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We report the synthesis and characterization of Zn-doped InN nanorods by metal-organic chemical vapor deposition. Electron microscopy images show that the InN nanorods are single-crystalline structures and vertically well-aligned. Energy-dispersive X-ray spectroscopy analyses suggest that Zn ions are distributed nonhomogenously in InN nanorods. Simulations based on diffusion model show that the doping concentration along the radial direction of InN nanorod is bowl-like from the exterior to the interior, the doping concentration decreases, and Such dopant distribution result in a bimodal EDXS spectrum of Zn across the nanorod. The study of the mechanism of doping effect is useful for the design of InN-based nanometer devices. Also, high-quality Zn-doped InN nanorods will be very attractive as building blocks for nano-optoelectronic devices.'

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Well-aligned Zn1-xMgxO nanorods and film with Mg-content x from 0 to 0.051 have been successfully synthesized by metal organic chemical vapor deposition (MOCVD) without any catalysts. The characterization results showed that the diameters and lengths of the nanorods were in the range of 20-80 nm and 330-360 nm, which possessed wurtzite structure with a c-axis growth direction. As the increase of Mg precursor flows into the growth chamber, the morphology of Zn1-xMgxO evolves from nanorods to a film with scale-like surface and the height of the nanorods and the film was almost identical, it is suggested that the growth rate along the c-axis was hardly changed while the growth of six equivalent facets of the type {1 0 (1) over bar 0} of the Zn1-xMgxO has been improved. Photoluminescence and Raman spectra show that the products have a good crystal quality with few oxygen vacancies. With the Mg incorporation, multiple-phonon scattering become weak and broad, and the intensities of all observed vibrational modes decrease. And the ultraviolet near-band-edge emission shows a clear blueshift (x=0.051, as much as 90 meV) and slightly broadening compared with that of pure ZnO nanorods. (C) 2008 Elsevier B.V. All rights reserved.

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We have investigated the optical properties of AlGaN grown on sapphire. It is found that two main luminescence peaks occur in the cathodoluminescence (CL) spectra of AlGaN films, and their energy separation increases with the increase of Al source flux during the growth. Spatially resolved CL investigations have shown that the line splitting is a result of variation of AlN mole fraction within the layer. The Al composition varies in both lateral and vertical direction. It is suggested that the difference in the surface mobility of Al and Ga atoms, especially, its strong influence on the initial island coalescence process and the formation of island-like regions on the uneven film surface, is responsible for the Al composition inhomogeneity. (C) 2008 Elsevier B.V. All rights reserved.

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The strain state of 570nm AlXGa1-xN layers grown on 600nm GaN template by metal organic chemical vapor deposition was studied using Rutherford backscattering (RBS)/channeling and triple-axis X-ray diffraction measurements. The results showed that the degree of relaxation (R) of AlxGa1-xN layers increased almost linearly when x less than or equal to 0.42 and reached to 70% when x = 0.42. Above 0.42, the value of R varied slowly and AI(x)Ga(1-x)N layers almost full relaxed when x = 1 (AIN). In this work the underlying GaN layer was in compressive strain, which resulted in the reduction of lattice misfit between GaN and AlxGa1-xN, and a 570nm AlxGa1-xN layer with the composition of about 0.16 might be grown on GaN coherently from the extrapolation. The different shape of (0004) diffraction peak was discussed to be related to the relaxation. (C) 2004 Elsevier B.V. All rights reserved.