草酸钴制备中的形貌继承性初探

在脉冲电磁场(PEMF)作用下,以氯化钴为母液、草酸铵为沉淀剂,采用草酸盐沉淀法制备了草酸钴粉体。利用扫描电子显微镜(SEM)对反应物及产物的形貌进行了表征,研究了反应产物与反应物之间的形貌继承性,并初步探索了草酸钴制备中的形貌继承机制。结果表明,在草酸盐沉淀法制备草酸钴的过程中,沉淀剂(父相)草酸根所承载的遗传信息在产物的显性性状中表现相对较弱,产物更多地继承了其母液(母相)氯化钴的形貌特征。脉冲电磁场作用造成的反应物形貌的改变,可以通过反应将此信息传递给产物,并使母相的形貌遗传作用加倍凸显出来。     

钯纳米颗粒的形貌控制合成

为优化钯纳米颗粒的化学还原法制备工艺,本文以氯钯酸(H₂PdCl₄)为前驱体,抗坏血酸(C₆H₈O₆)为还原剂,聚丙烯酸钠(PAAS)为表面活性剂制备钯纳米颗粒。采用正交实验探究不同工艺参数对钯纳米颗粒粒径和形貌的影响。通过 X射线粉末衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)及电化学工作站对制备产物的结构、物相、形貌、电催化性能进行了表征。结果表明:在相同的工艺体系下,通过温度的改变,40 ℃条件下可以得到粒径大小为64.5 nm,球形度较好,分散性高的钯纳米颗粒;90 ℃条件下可以得到粒径大小为45.9 nm的立方体钯纳米颗粒。所制备的球形和立方体钯纳米颗粒对甲酸的电氧化催化活性分别为商业钯黑的1.57倍和1.49倍,在催化剂制备领域有广泛的应用前景。     

Fe_xNi_(1-x)合金粉的制备及吸波性能

采用草酸盐沉淀-前驱体热分解法制备不同成分的Fe_xNi_(1-x)(0x1)合金粉。采用XRD和SEM分别测试前驱体和合金粉的物相结构与形貌。结果表明:随着Ni含量增大,前驱体物相由FeC_2O_4·2H_2O逐渐向NiC_2O_4·2H_2O转变,形貌由短棒状向立方体、多面体转变。Fe_xNi_(1-x)合金粉的几何外形与前驱体基本一致,但结构上呈多孔状,且粒径变小。Fe_xNi_(1-x)合金粉的物相结构随其成分变化,由富铁的bcc结构向富镍的fcc结构转变。测试不同成分Fe_xNi_(1-x)合金粉与石蜡复合物的电磁参数,并计算其吸波性能,Fe0.5Ni0.5具有最大的电磁损耗能力,厚3.0mm时在6.82GHz处具有最小反射损耗RL,为-52.58dB。Fe0.6Ni0.4具有最大有效频宽,厚1.5mm时反射损耗小于-10dB的有效频宽达4.02GHz。     

室温固相反应制备纳米Co_3O_4粉体

以硝酸钻和碳酸氢铵为原料,采用室温固相反应首先制备出前驱物碱式碳酸钴,然后将前驱物在２５０℃分解３ｈ,得到纳米四氧化三钴．用Ｘ射线粉末衍射、透射电镜、热分析仪、扫描电镜对产物的组成、大小、形貌及有关性质进行了表征．结果表明获得了平均粒径在13nm、分布均匀、无团聚的纳米粉体．     

室温固相反应制备纳米Co3O4粉体

以硝酸钴和碳酸氢铵为原料,采用室温固相反应首先制备出前驱物碱式碳酸钴,然后将前驱物在250℃分解3h,得到纳米四氧化三钴,用X射线粉末衍射、透射电镜、热分析仪、扫描电镜对产物的组成、大小、形貌及有关性质进行了表征。结果表明获得了平均粒径在13nm,分布均匀、无团聚的纳米粉体。     

纳米TiO2薄膜的制备及其表面形貌AFM观测

采用溶胶-凝胶法在玻璃载波片及ITO导电玻璃片上制备出负载型纳米TiO2薄膜,并用原子力显微镜(AFM)对不同条件下制备的TiO2的表面形貌进行了表征.结果表明,TiO2薄膜能较好地负载在玻片表面,并且TiO2薄膜的表面形貌与前驱物的配比浓度、基片、热处理温度等都有密切的关系.随浓度和镀膜层数的增大,薄膜中TiO2纳米微晶的颗粒尺寸逐渐增大,从细小均匀粒子膜变为较大不规则的板块结构.在ITO薄膜面形成的TiO2薄膜具有较小的颗粒和均匀的分布.     

液相法制备条件对钴粉形貌和电化学性能的影响

在室温下用液相还原法制备了单质钴粉末。采用XRD和SEM分析了粉末的相结构和微观形貌,并研究了表面活性剂的种类及浓度、钴源浓度和还原剂浓度对粉末最终形貌的影响。结果表明,引入PVA作为表面活性剂时,有利于形成球状结构,且PVA浓度越大,颗粒尺寸越小,颗粒分布越均匀。当PVA浓度为0.5%,水合肼浓度为80%,Co~(2+)浓度为2.5M时,所得样品呈花球状结构。恒流充放电测试结果表明,由该钴粉制备的电池负极材料样品具有较高的放电容量,最高可达533mAh/g,且高倍率放电能力良好,1500mA/g的电流密度下放电容量能达到331.4mAh/g。     

水热法一步合成VO2粉末及其微观形貌调控

采用水热法,钒源选择V_2O_5,在使用还原剂草酸,不使用其他表面活性剂及模板的条件下,制备了具有不同微观形貌的VO_2(B)和VO_2(M)粉末,主要研究了草酸溶液浓度变化对产物微观形貌的影响。利用X射线衍射仪(XRD)对粉末的晶型结构和物相组成进行分析,通过扫描电子显微镜(SEM)对粉末的微观形貌进行表征。在180℃水热反应温度下,制备出了具有多种特殊微观形貌的VO_2(B)粉末,典型的如"雪花"状、"杨桃"状以及均匀短棒状等,全面系统地对粉末所出现的不同微观形貌进行了总结。采用蓝电电池测试系统对不同微观形貌VO_2(B)粉末制备的锂离子电池进行充放电测试,结果表明,"杨桃"状VO_2(B)锂离子电池性能较优,比容量峰值可达4 683.8mAh/g,但电池循环特性较差。同时,在水热反应温度260℃下,合成了微观形貌分别为短棒状、"雪花"状、"核桃"状以及球状的VO_2(M)粉末。DSC测试结果显示,VO_2(M)粉末形貌对其相变温度影响较小。     

钨粉颗粒形貌对钨铜合金药型罩破甲性能的影响

为了研究钨粉形貌对钨铜合金药型罩破甲性能的影响,采用了4种不同颗粒形貌的钨粉,利用机械合金化法和冷等静压旋压工艺制备钨铜合金药型罩,并对钨铜合金药型罩射孔弹进行了地面静破甲穿钢靶试验,通过试验分析钨粉形貌对钨铜合金药型罩破甲性能的影响。结果表明:钨粉颗粒完整、形貌为多面体的钨粉,其松装密度达到9.564 g/cm~3,制备的钨铜合金药型罩的破甲深度达到338.3 mm,破甲稳定性达到99.21%;而钨粉颗粒有缺陷、形貌为类球状的钨粉,其松装密度仅为7.142 g/cm~3,制备的钨铜合金药型罩的破甲深度为288.1 mm,破甲稳定性为92.7%,分别下降了17.4%和7.6%。     

钨粉颗粒形貌对钨铜合金药型罩破甲性能的影响

为了研究钨粉形貌对钨铜合金药型罩破甲性能的影响,采用了4种不同颗粒形貌的钨粉,利用机械合金化法和冷等静压旋压工艺制备钨铜合金药型罩,并对钨铜合金药型罩射孔弹进行了地面静破甲穿钢靶试验,通过试验分析钨粉形貌对钨铜合金药型罩破甲性能的影响。结果表明:钨粉颗粒完整、形貌为多面体的钨粉,其松装密度达到9.564 g/cm³,制备的钨铜合金药型罩的破甲深度达到338.3 mm,破甲稳定性达到99.21%;而钨粉颗粒有缺陷、形貌为类球状的钨粉,其松装密度仅为7.142 g/cm3,制备的钨铜合金药型罩的破甲深度达到338.3 mm,破甲稳定性达到99.21%;而钨粉颗粒有缺陷、形貌为类球状的钨粉,其松装密度仅为7.142 g/cm³,制备的钨铜合金药型罩的破甲深度为288.1 mm,破甲稳定性为92.7%,分别下降了17.4%和7.6%。     

Similarity between craze morphology and shear-band morphology in polystyrene

The formation of shear bands and crazes in thin films as well as in bulk samples of polystyrene were examined in the electron microscope using a variety of replication techniques. The morphologies of shear bands and crazes are quite similar both depending initially upon the relative shear displacement of 400 to 1000 Å domains. As deformation continues and orientation increases, fibrils varying from 50 to 700 Å are formed within the deformation zone, lateral constraint of the normal Poisson contraction causing voids to form in the crazes but not in the shear bands. Shear-band width was found not to be a unique function of either temperature or strain-rate and both craze and shear-band morphologies were found not to be strong functions of molecular weight. Regardless of molecular weight, fibrils formed within the deformation zone were always on the order of a few hundred Angstroms in diameter. However, for thin films of molecular weight less than 20 000 insufficient numbers of tie molecules between fundamental structural units or domains made it difficult for these fibres to span the craze width.     

Computer prediction of crystal morphology

Control of crystal shape is of great importance to several contemporary industries and thus there is a need to understand the fundamental processes determining crystal morphology. Computer simulations have been widely used in an attempt to predict the morphology of crystals in real systems under a variety of conditions and this review demonstrates that great strides have been made in this area over the last 18 months.     

Wax morphology in bitumen

Wax crystallisation and melting in bitumen is usually considered detrimental to bitumen quality and asphalt performance. The objectives of this paper are to study wax morphology in bitumen and to investigate effects of time, temperature, and thermal cycling on wax crystallisation. Various samples were selected, including eight waxy bitumens of different sources and three laboratory blends prepared by adding a slack wax and two isolated bitumen waxes to the non-waxy bitumen. Test methods used were differential scanning calorimetry (DSC), polarised light microscopy (PLM), confocal laser scanning microscopy (CLSM), and freeze etching (fracture) in combination with transmission electron microscopy (FF-TEM). The DSC results indicated that the selected bitumen samples differ widely in wax content and wax crystallisation starting and melting out temperatures. It was found that non-waxy bitumen displayed no structure or crystals neither in PLM, CLSM or FF-TEM, while waxy bitumens from different crude origins showed a large variation of structures. The morphology of wax crystals was highly dependent on crystallisation temperature as well as temperature history. The wax which has been isolated from waxy bitumen and mixed into non-waxy bitumen displayed similar morphology as the wax in the original bitumen. It was also found that bitumen wax usually melted at temperatures lower than 60°C although in one case a temperature of 80°C was needed until complete melting of the wax.     

Fine-scale morphology of ultraviolet-ozone etched polyethylene

The process of ablation of the surface of polyethylene using ultraviolet radiation in the presence of ozone has been studied. The average rate of material erosion is quite small but is selective, preferentially etching the amorphous regions. The resultant fine scale surface topography has been examined using transmission electron microscopy of replicas, and lamellae are readily visible. The light source emitted two principal wavelengths, with the shorter wavelength affecting measured etching rates more strongly.     

Preparation of an ultra-oriented polyethylene morphology

A technique for producing an ultra-drawn morphology for high-density polyethylene has been described previously. This technique has subsequently been extensively modified to produce the ultra-drawn morphologies under continuous and more versatile conditions. These changes involve using the reservoir of an lnstron rheometer to prepare a crystal morphology prior to proceeding with a solid state (crystal-crystal transformation) extrusion process in the same instrument. The new preparation conditions are described to up-date the prior procedure and to document this new method which is now being employed in several laboratories to produce transparent polyethylene morphologies of extreme orientation and chain extension which results in filaments and films of extreme tensile moduli.     

Aggregation morphology of synthetic peptidic amphiphiles

Peptidic amphiphiles containing various homo-oligopeptides were synthesized. Their aggregation morphologies in aqueous dispersion were studied using dark-field optical microscopy. The amphiphile containing three glycine residues formed amorphous precipitates. The amphiphile containing three sarcosine residues formed novel twisted ribbon-like aggregates with a long pitch (15–25 μm). The amphiphile containing three proline residues formed fibrous helical superstructures (50–70 μm in length). The last two morphologies were stable only at temperatures below the phase transition temperature. Different aggregation morphologies of the peptidic amphiphiles in aqueous dispersion were observed in the presence and absence of amide (NH) protons. Small amounts of additives altered the morphological structure of the aggregates on incubation.     

报废管板大锻件中的夹杂物形貌研究

为了提高管板大锻件的成品率,采用低倍和高倍检验、扫描电镜及微区成分分析等方法,研究了报废管板大锻件中夹杂物的形貌及性质.研究表明:报废管板中含有大量的片状夹杂物,管板的缺陷性质为夹杂性穿晶裂纹,具有氢脆特性.     

Purity and morphology of aluminium films

A continuous wire feed source of aluminium of 99.999% purity in conjunction with a composite ceramic boat has been used to deposit aluminium films of high purity in vacuum. The impurity content was analysed by proton-induced X-ray analysis with a Van de Graaff accelerator, supplemented by X-ray fluorescence, optical emission and Auger electron spectroscopy. The low impurity content achieved ( 50 atomic ppm) is attributed to the small quantity of molten aluminium maintained in the boat at one time.

The morphology of the Al films was studied by reflection electron diffraction, X-ray diffraction and scanning electron microscopy. Thick Al films grew with {111} and {311} texture orientations. The grain size variation with thickness generally followed the known variation with the deposition rate.     

Predicting the morphology of nanostructured composites

The mixing of microphase-separating diblock copolymers and nanoparticles can lead to the self-assembly of organic/inorganic hybrid materials that are spatially organized on the nanometer length scale. There is a considerable challenge in modeling such systems since the appropriate theories must capture not only the formation of the diblock mesophases but also the copolymer–particle and particle–particle interactions, which can affect the ultimate structure of the material. Recently, a theoretical approach has been developed to describe the behavior of diblock/particle mixtures and predict the equilibrium morphology of the resulting composites. The approach, which combines self-consistent field and density functional theories, can facilitate the design of hybrid materials with the desired morphology for novel opto-electronic devices, separation membranes and catalysts.