Magnetic properties,phase evolution,hollow structure and biomedical application of hematite (α-Fe2O3) and QUAIPH

We investigate synthesis, phase evolution, hollow and porous structure and magnetic properties of quasi-amorphous intermediate phase (QUAIPH) and hematite (α-Fe₂O₃) nanostructure synthesized by annealing of akaganeite (β-FeOOH) nanorods. It is found that the annealing temperature determines the phase composition of the products, the crystal structure/size dictates the magnetic properties whereas the final nanorod morphology is determined by the starting material. Annealing of β-FeOOH at ～300 °C resulted in the formation of hollow QUAIPH nanorods. The synthesized material shows low-cytotoxicity, superparamagnetism and good transverse relaxivity, which is rarely reported for QUAIPH. The QUAIPH nanorods started to transform to porous hematite nanostructures at ～350 °C and phase transformation was completed at 600 °C. During the annealing, the crystal structure changed from monoclinic (akaganeite) to quasi-amorphous and rhombohedral (hematite). Unusually, the crystallite size first decreased (akaganeite → QUAIPH) and then increased (QUAIPH → hematite) during annealing whereas the nanorods retained particle shape. The magnetic properties of the samples changed from antiferromagnetic (akaganeite) to superparamagnetic with blocking temperature T_B = 84 K (QUAIPH) and finally to weak-ferromagnetic with the Morin transition at T_M = 244 K and high coercivity H_C = 1652 Oe (hematite). The low-cytotoxicity and MRI relaxivity (r₂ = 5.80 mM^?1 s^?1 (akaganeite), r₂ = 4.31 mM^?1 s^?1 (QUAIPH) and r₂ = 5.17 mM^?1 s^?1 (hematite)) reveal potential for biomedical applications.     

Synthesis of manganese titanate and its precursors from xerogel

An overview of research on the synthesis of manganese titanates is presented. The xerogel of Mn–Ti–O–C–H composition was synthesized from manganese acetate and titanium tetrabutylate via liquid-phase method using organic solvents. The calcination of xerogel in air at 450 °C and 700 °C yielded manganese titanate precursors in the form of a nanostructured mixture of Mn₂O₃ and TiO₂. Annealing at 1000 °C, manganese metatitanate MnTiO₃ was obtained. Reference experiments with initial reagents included, separately, thermal decomposition of Mn(CH₃COO)₂×4H₂O and the product of Ti(OC₄H₉)₄ hydrolysis. The composition, structure, and properties of the products were studied using X-ray diffraction, scanning electron microscopy, elemental analysis, diffuse reflectance IR Fourier spectroscopy, thermogravimetry, and by measuring specific surface area. The data presented by these different techniques are basically consistent with each other (with an increase in the annealing temperature, an increase in globule size and decrease in specific surface area are observed; structuring occurs within the long- and short-range order; the size of the crystallites does not exceed that of the globules; elemental composition correlates with phase composition; the endothermic character of the reaction of MnTiO₃ formation at 900 °C is confirmed by a thermodynamic calculation). Nevertheless, some unexpected effects were revealed (based on the FTIR diffuse reflection spectra, mixed oxide Mn–Ti–O is formed in the surface layer of particles already at 450 °C and 700 °C; etc.). Application of the proposed technique for modifying Al₂O₃ powders, with the aim of implementing low-temperature sintering of corundum ceramics, is discussed.     

Fluoride-mediately solvothermal synthesis and tunable photocatalytic selectivity of urchin-like ZrO2 hollow microspheres

Photocatalysts often show excellent performances on the basis of their surface state of exposed faces with high reactivity, but unfortunately surfaces of this type are usually concealed into the interior of crystals for their high surface energy. We report here a possibility that for fluorine-terminated surfaces of monoclinic ZrO₂, these higher-energy surfaces could be retained and exposed. Urchin-like ZrO₂ hollow microspheres (UZHS) composed of nanoribbons with exposed (010) facets are obtained through a fluoride mediately solvothermal method. We prove the stabilization effect of fluorine adsorption on (010) facets by density functional theory calculations. More interestingly, UZHS exhibit tunable photocatalytic selectivity in dye degradation. The fluorinated UZHS exhibit good performances both on decomposing Congo red (CR) and methylene blue, while the surface-modified UZHS by calcination only favor decomposition of CR.     

Molten salt synthesis of MAX phases in the Ti-Al-C system

The molten salt method was used to synthesise the MAX phase compounds Ti₂AlC and Ti₃AlC₂ from elemental powders. Between 900–1000?°C, Ti₂AlC was formed alongside ancillary phases TiC and TiAl, which decreased in abundance with increasing synthesis temperature. Changing the stoichiometry and increasing the synthesis temperature to 1300?°C resulted in formation of Ti₃AlC₂ alongside Ti₂AlC and TiC. The type of salt flux used had little effect on the product formation. The reaction pathway for Ti₂AlC was determined to be the initial formation of TiC_1-x templating on the graphite and titanium aluminides.     

氰酸钾合成研究进展

综述了氰酸钾的合成方法,并对各种方法进行了评价,其中液固相反应法具有原料易得,操作简便,产物纯度较高、易与溶剂分离、经济性好等特点,适用于工业化生产。     

DCPD和PET合成不饱和聚酯的研究

探讨了用双环戊二烯和聚对苯二甲酸乙二醇酯废料合成不饱和聚酯树脂的方法：PET用二元醇醇解后，加入顺入烯二酸酐和DCPD，在80－120℃条件下滴加与DCPD等量的水进行反应，反应大约2.5h，加入其它成分，升温酯化直至反应完全。PET一定时，DCPD的含量影响不饱和聚酯同苯乙烯的互溶性和固化过程，DCPD和PET合成的不饱和聚酯树脂与标准树脂相比较，机械性能好，空干性好，解决了环境污染，具有很好的经济效益。     

Synthesis,characterization and ion exchange properties of zirconium(IV) tungstoiodophosphate,a new cation exchanger

Zirconium(IV) tungstoiodophosphate has been synthesized under a variety of conditions. The most chemically and thermally stable sample is prepared by adding a mixture of aqueous solutions of 0·5 mol L⁻¹ sodium tungstate, potassium iodate and 1 mol L⁻¹ orthophosphoric acid to aqueous solution of 0·1 mol L⁻¹ zirconium(IV) oxychloride. Its ion exchange capacity for Na⁺ and K⁺ was found to be 2·20 and 2·35 meq g⁻¹ dry exchanger, respectively. The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the exchange capacity of drying the exchanger at different temperatures has been studied. The analytical importance of the material has been established by quantitative separation of Pb²⁺ from other metal ions.     

Interval based MINLP superstructure synthesis of mass exchange networks

A new simultaneous synthesis approach for mass exchange networks (MENs) is presented. The technique is adapted from the interval based mixed integer non-linear program (MINLP) superstructure (IBMS) synthesis of heat exchanger networks (HENs). The superstructure interval boundary compositions are defined by the supply and target compositions of either the rich or lean set of streams. Each rich and lean stream in the superstructure has the potential of exchanging mass with streams of opposite kind in each interval based on mass transfer feasibility. The model harnesses the strengths of the stagewise superstructure and the pinch technology methods for mass exchange network synthesis (MENS). The IBMS approach simultaneously trades-off the capital and operating costs for MENs. The superstructure composition interval defining approach introduced in this paper enforces the mixing of split streams at equal compositions, hence there is no need to include mixing equations in the model. Fixing the interval boundaries helps to eliminate the complexities involved in initialisations, thus the region of search for the optimum solution is reduced. The IBMS model is applied to MENS problems involving continuous contact and staged columns. It is also extended to problems involving multiple mass separating agents (MSAs) and regeneration. The results obtained compare well with those in the literature.     

Synthesis and Hydrogen Storage in Single—walled Carbon Nanotubes

Single=walled carbon nanotubes(SWNTs) were synthesized by a hydrogen arc discharge method.A high yield of gram quantity of SWNTs per hour was achieved.Tow kinds of SWNT products:web-like substancea and thin films in large slices were obtained. Results of resonant Raman scattering measurements indicate that the SWNTs prepared have a wider diameter distribution and a larger mean diameter.Hydrogen uptake measurements of the two kinds of SWNT samples(both as prepared and pretreated) were carried out using a high pressure volumetric method,respectively.And a hydrogen storage capacity of 4 wt pct could be repeatedly achieved for the suitably pretreated SWMNTs,whicb indicates that SWNTs may be a promising hydrogen storge material.     

聚碳硅烷的分子量分布与可纺性研究

阐述了聚碳烷的合成及其分子量分布，讨论了高低分子含量对聚碳硅烷熔点及可纺性的影响，而且提出了分子量分布的控制标准与方法。