碳铵尿素双沉淀法合成球形纳米 α-Al2O3粉体的研究

报道了一种用硝酸铝和碳酸铵以及尿素反应制备球形纳米α-Al2O3粉体的便捷方法.通过X射线粉末衍射、差热分析和扫描电镜对产物进行表征观察,结果显示,用这种方法所合成的前驱体为2～6μm鹅卵石形状的氢氧化铝.前驱体再经1200℃煅烧2 h得到直径为200 nm左右的孪生球形纳米氧化铝粉体.在此过程中,尿素起到了调节形貌的作用.     

纳米SiO2对可水合氧化铝水化行为及流变性的影响

研究了纳米SiO2对可水合氧化铝水化行为的影响以及纳米SiO2与可水合氧化铝混合料浆的流变性.利用XRD和SEM,研究了水化产物的物相组成和形貌特征,并利用Zeta电位仪与流变仪,测试了纳米SiO2-可水合氧化铝料浆的表面电位与流变行为.结果表明:纳米SiO2的添加减缓了可水合氧化铝的水化速度,其原因是纳米SiO2在可水合氧化铝颗粒表面形成包覆层阻碍了其与水的直接接触,从而降低了可水合氧化铝的水化速率;在碱性条件下,纳米SiO2的添加使可水合氧化铝料浆具有良好的分散性,降低了料浆的触变性,使料浆呈现剪切变稀行为.     

用电沉积法在氧化铝模板中制备氧化锌纳米线的研究

利用直流电沉积法在阳极氧化铝模板的有序孔洞中生长了氧化锌纳米线,首次在氧气氛围中将锌氧化成氧化锌.用场发射扫描电子显微镜(FE-SEM)和X射线衍射仪(XRD)对其形貌及成分进行表征和分析.结果表明,氧化铝模板的有序孔洞中填充了高致密、均一连续的锌纳米线.在氧气氛围中,800 ℃下氧化2 h,氧化铝中的锌纳米线己全部氧化成氧化锌纳米线.光致发光光谱表明,氧化锌纳米线在496 nm处有较强蓝绿光发射.     

醇-水体系中pH值和焙烧温度对合成MgO纳米片晶体性质的影响

采用液相法,在醇-水体系中,以Mg(NO3)2·6H2O为镁源、PEG-2000为表面活性剂、NH3·H2O为沉淀剂,研究了pH值和焙烧温度对制备MgO纳米片晶体性质的影响.采用XRD、SEM和BET等手段对MgO纳米片晶相组成、微观形貌、孔结构进行分析表征.研究结果表明,pH值和焙烧温度对MgO纳米片晶相组成没有影响,但对样品微观形貌和比表面积影响较大.较低的pH值和焙烧温度或者较高的pH值和焙烧温度均会导致样品形状不规则,出现不同程度团聚,比表面积较小.在pH=10、焙烧温度500℃条件下制得MgO纳米片形状规整、分散性较好,比表面积、孔容和平均孔径分别为145.42 m2·g-1、0.67 mL·g-1和18.56 nm.     

Er3+离子在多孔模板内的发光特性

利用两次阳极氧化的方法制备多孔氧化铝模板，然后采用溶胶-凝胶法将铒的乙酰丙酮配合物掺人多孔氧化铝的模板内，制得了Er3 离子的SiO2凝胶。用扫描电镜(SEM)观察了多孔氧化铝模板的形貌，并测试了乙酰丙酮合铒的红外吸收谱以及Er3 离子在多孔模板内的室温荧光谱。初步结果显示纳米孔洞导致了荧光峰变窄。     

片状纳米氧化锌单晶的制备和表征

本文提供了一种应用二步法制备片状纳米氧化锌单晶的实验方法--首先,以尿素为沉淀剂宿主,以氯化锌、碱式碳酸锌为原料,应用均匀沉淀法获得纳米氧化锌的片状纳米级前驱物;然后通过控温热分解前驱物制备出片状纳米氧化锌单晶.用扫描电镜观测了制备的ZnO单晶的形貌,并通过红外光谱对其进行了表征.结果表明:实验制备的氧化锌均为无色透明的片状单晶,结晶形貌为正六边形、五边形、矩形以及其它不规则形状,单晶直径在30～600μm之间,厚30～60nm;影响纳米氧化锌单晶制备的主要因素是反应物料配比、沉淀剂宿主尿素的浓度(1∶6)以及反应温度(70～85℃).此外,乙醇的含量对片状纳米前驱物的形貌影响很大,10;～40;的乙醇含量利于形成片状纳米氧化锌单晶.     

核壳结构Fe3 O4@ZnO纳米粒子的制备及电磁波吸收性能研究

结合溶剂热法和溶胶-凝胶法制备出核壳结构的Fe3 O4@ZnO纳米粒子,通过TEM、SEM、XRD、VSM和矢量网络分析仪对材料的形貌、微观结构、磁性能和电磁波吸收特性进行了表征.结果表明,制备得到的Fe3 O4@ZnO纳米粒子核壳结构明显,形状规整,属于铁磁性材料,并且ZnO壳层的厚度直接影响到Fe3 O4@ZnO纳米粒子的电磁波吸收效果.     

微波熔盐沉积制备AlN纳米晶及光致发光特性研究

以高纯AlCl3和Li3N为反应原料,NaCl和KCl为混合熔盐,使用微波熔盐沉积法在700℃制备出A1N纳米晶.利用XRD、SEM、EDS等对纳米晶的物相、形貌进行了定性和定量表征,并使用PL测试了材料的光学性质,分析了主要缺陷类型.XRD测试结果表明,实验获得产物为六方纤锌矿结构的AlN.使用Scherrer公式估算了AlN 产物的晶粒平均粒度大小约为35.6 nm,表明所得确为AlN纳米晶.SEM观测到的纳米晶形貌为方形,分布均匀且晶粒形状几近,平均粒度约为35 nm.EDS测试结果显示AlN纳米晶中Al和N的原子相对百分含量为50.521;和49.479;,其化学配比几近于1∶1物质的量比.室温PL测试发现发光中心在435 nm,缺陷主要是杂质缺陷类型.以上结果充分表明微波熔盐沉积法是一种制备AlN纳米晶的有效方式.     

片状纳米氧化锌单晶的制备和表征

本文提供了一种应用二步法制备片状纳米氧化锌单晶的实验方法--首先,以尿素为沉淀剂宿主,以氯化锌、碱式碳酸锌为原料,应用均匀沉淀法获得纳米氧化锌的片状纳米级前驱物;然后通过控温热分解前驱物制备出片状纳米氧化锌单晶.用扫描电镜观测了制备的ZnO单晶的形貌,并通过红外光谱对其进行了表征;讨论了溶液中生成纳米氧化锌的前驱物的热力学趋势,并对氧化锌制备过程进行了结晶动力学分析.结果表明:实验制备的氧化锌均为无色透明的片状单晶,结晶形貌为正六边形、五边形、矩形以及其它不规则形状,单晶直径在3～30μm之间,厚30～60nm;影响纳米氧化锌单晶制备的主要因素是反应物料配比、沉淀剂宿主尿素的浓度(1∶6)以及反应温度(70～85℃).此外,乙醇的含量对片状纳米ZnO前驱物的形貌影响很大,过高(＞40;)或过低(＜10;)的乙醇含量都不利于形成片状纳米氧化锌单晶的前驱物.     

纳米分散颗粒Li1.2Ni0.2Mn0.6O2材料的制备及性能

以乙酸盐和一水合柠檬酸为原料,采用溶胶-凝胶法合成锂离子电池纳米级富锂锰基正极材料Li1.2 Ni0.2 Mn0.6 O2.X射线衍射(XRD)结果显示所得产物为结晶度良好、离子混排程度低的纯相结构材料;扫描电镜(SEM)结果显示所得材料为纳米颗粒(颗粒直径均在300 nm以内),且具有圆形或者正六边形形状结构,表面光滑,粒度分布均匀.研究了高温焙烧温度对Li1.2 Ni0.2 Mn0.6 O2材料结构形貌及电化学性能的影响,重点探讨了结构形貌对电化学性能的影响规律.实验结果表明:当焙烧温度为850℃和900℃时,材料的形貌结构更好,电化学性能更为理想.     

Science for the small and the tall,the young and the old

Public engagement becomes increasingly important for scientists. One reason is the demand of the taxpayer to know what her or his money is being spent on, and why. The other one is that in a world that increasingly relies on technology, student engagement even at a very young age becomes a target to assure the needed supply of well-educated and especially motivated scientists for the decades to come. And it falls on the older generation of current researchers to leave the comfort of their lab once in a while, to awaken the interest for science among the population. Many people may know that there is a ‘liquid crystal’ in their mobile (cell) phone display, but when prompted, no one really knows what that liquid crystal actually is, let alone how the display they use many times every day, actually works in principle. It is part of our job to change this. In this contribution Valentina Domenici and Ingo Dierking would like to report on two recent Science Festival events in which they took part, one held in Genoa, Italy, and the other in Manchester, UK.     

On the role of the porous shell of the solid core of the earth in the anomalous heat and mass flow to the mantle

The model of the pressure-induced first-order phase transition of a metal melt to the metallicglass state considers a thermodynamically nonequilibrium porous near-surface shell of the solid core of the Earth, which contacts cyclonic vortices in the liquid core. Anomalous flows of heat and light-material mass to the mantle from the solid core at these contact points are calculated. These anomalous flows are shown to be comparable with the observed ones under the assumption of a rapid increase in the melt viscosity at pressures of 1–10 Mbar, which is characteristic of a solid core. In this case, the porous layer permeability may be very low.     

On the dependence of the surface tension at the crystal-melt interface on the impurity concentration

The stationary task of impurity diffusion in a melt has been solved within a two-dimensional crystallization model in a second-order approximation with respect to the amplitude of deviation from a smooth crystallization front. The dependence of the surface tension Γ at the interface on the impurity concentration C is taken into account in the form Γ = Γ₀ + ζ _d C, where Γ₀ and ζ _d are constants. The variational method is used to obtain the condition for the transition from a smooth crystallization front to a cellular one. It is shown that calculated cell sizes are in agreement with the experimental data in the literature only when the parameter ζ _d ≠ 0. For binary systems with distribution coefficients k < 1 and k > 1, ζ _d should be positive and negative, respectively.

     

On the inhomogeneity of the transition surface layer of the solid core of the earth

Different geophysical data and conclusions of theoretical models, which can give information about the behavior of the solid and liquid cores of the Earth as well as about the existence of a transition layer as a temperature-hysteresis region at a relatively weak first-order phase transition, are compared. It is concluded that liquid inclusions inevitably exist in this region; these inclusions are involved (due to the complex convective processes occurring in the liquid core) in the transport of light materials from some areas of the solid-core surface. The porosity and permeability of the transition layer determine the seismic acoustic inhomogeneities in these areas, which contact the convective flows in the liquid core. In particular, this explains the well-known ??east-west?? effect. Obviously, the model of the crystalline core is not the only possible alternative for a model of a core with a metallic glasslike structure.     

On the entropy difference between the vitreous and the crystalline state

The paper deals with the entropy difference between frozen-in phases and their equilibrium counterparts. First, the nature of data compiled in thermochemical data collections are briefly reviewed, comprising data for non-equilibrium phases. Then, experimental evidence from earlier literature is compiled showing that the conventional entropy of a frozen-in phase at zero Kelvin assumes a non-zero residual value S(0). Based on calorimetric data from multiple sources, the same evidence is elaborated for diopside glass, yielding S_glass(0) = 24.8 ± 3 J/(mol K), a value reproducing a result publishes earlier. The zero Kelvin enthalpy of this glass is H_glass(0) = 81±8 kJ/mol. For S_glass(0), a structural interpretation in terms of silicate chain mixing is proposed, yielding a lower threshold for S_glass(0). From the point of view of statistical mechanics, non-zero residual entropies of frozen-in phases can be derived from ensemble averages, however, not from time averages.     

二价阳离子掺入KDP晶体能力的研究

本文旨在寻找影响杂质阳离子进入KDP晶体能力的因素,我们使用分析纯的KH2PO4和超纯水(电阻率≥18.2MΩ·cm)为原料,分别加入BaCl2·2H2O,CuCl2·2H2O和MgCl2·6H2O,通过降温方式快速生长出KDP晶体.结果表明,cu2+及Mg2+在晶体中的含量基本保持不变,不随其在生长溶液中量的增大而增大,cu2+在晶体中的含量大于Mg2+在晶体中的含量;不同的是,Ba2+在晶体中的含量随着其在生长溶液中量增大而增大.从实验结果我们推断出离子半径和离子水合热是影响二价杂质阳离子在水溶液晶体生长过程中进入KDP晶体能力的重要因素.     

Investigations of the Chemical Composition of the Metal Finds from the Levadki Necropolis

Crystallography Reports - Copper-based alloy items of the III century A.D., found in Burial no. 182 of the Late-Scythian Levadki necropolis in the submountain Crimea, have been investigated. The...     

Effect of the temperature on the TMOS sono-hydrolysis and a study of the structure of the resulting aged sonogels

The effect of temperature on the oxalic acid catalyzed sono-hydrolysis of tetramethoxysilane (TMOS) was studied by means of a heat flux calorimetric method. The activation energy of the process was measured as (24.5 ± 0.8) kJ/mol in the temperature range between 10 and 50 °C. The structural characteristics of the resulting sonogels, after long period of aging in saturated conditions, were studied by means of small angle X-ray scattering. The structure can be described as formed by ∼2.7 nm mean size mass fractal-like aggregates (clusters) of primary silica particles of ∼0.3 nm mean size, all imbibed in a liquid phase. The average mass fractal dimension of the clusters was found to be 2.58. The primary particle density was estimated as 2.23 g/cm³, in good agreement with the value frequently quoted for fused silica. The volume fraction of the clusters in the saturated sonogels was estimated as about 28%. The moment in which the meniscus of the liquid phase penetrates into the clusters under rapid evaporation process has been detected by an inflection in the first derivative of the curve of weight loss in a simple thermogravimetric test.