Clogging behavior of submerged entry nozzles for Ti-bearing IF steel

The nozzle clogging behavior of Ti-bearing IF steel was studied by metallographic analysis, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD). According to the experimental results, nozzle clogging primarily appears three layers. There are a lot of large-sized iron particles in the inner layer and mainly slag phase in the middle and outer layers. The principal clog constituents of the inner layer are loose alumina cluster inclusions and granular shaped alumina inclusions, containing iron particles. The clog constituents of the middle layer are mainly dendrite alumina inclusions. The primary phases existing in nozzle clogging are FeO·TiO₂ and FeO·Al₂O₃ besides α-Al₂O₃ and α-Fe. The FeO·TiO₂ phases among the deposits adhere the deposits together firmly enough to lead to the inferior castability of Ti-bearing ultra low carbon steel compared with that of Ti-free low carbon Al-killed steel.     

Microstructure evolution and phase transformation of traditional cast and spray-formed hypereutectic aluminium-silicon alloys induced by heat treatment

Microstructural evolution and phase transformation induced by different heat treatments of the hypereutectic aluminium-silicon alloy, Al-25Si-5Fe-3Cu (wt%, signed as 3C), fabricated by traditional cast (TC) and spray forming (SF) processes, were investigated by differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) combined with energy dispersive X-ray spectroscopy and X-ray diffraction techniques. The results show that Al₇Cu₂Fe phase can be formed and transformed in TC- and SF-3C alloys between 802–813 K and 800–815 K, respectively. The transformation from β-Al₅FeSi to δ-Al₄FeSi₂ phase via peritectic reaction can occur at around 858–870 K and 876–890 K in TC- and SF-3C alloys, respectively. The starting precipitation temperature of δ-Al₄FeSi₂ phase as the dominant Fe-bearing phase in the TC-3C alloy is 997 K and the exothermic peak about the peritectic transformation of δ-Al₄FeSi₂→β-Al₅FeSi is not detected in the present DSC experiments. Also, the mechanisms of the microstructural evolution and phase transformation are discussed.     

MFI-type zeolite membrane on hollow fiber substrate for hydrogen separation

High performance MFI-type zeolite membranes on the outer surface of α-Al 2 O 3 hollow fibers were synthesized by secondary growth method using pure silica sol without an organic template. X-ray diffraction was used to characterize the phase structure of both the seed layer and zeolite membrane. The morphologies of the seed layer and zeolite membrane were examined by scanning electron microscopy. The zeolite membrane achieved an extraordinary H 2 /CO 2 separation factor of 10 with a high H 2 permeance of 5.56 10 -7 mol m -2 s -1 Pa -1 at 723 K.     

Synthesis of nonstoichiometric M-type barium ferrite nanobelt by spark plasma sintering method

This study investigated the feasibility of ultrafast crystallization of M-type barium ferrite when the coprecipitation precursors in stoichiometric proportions as BaFe12O19, Fe(OH)3 and BaCO3 nanoparticles, had been heated by spark plasma sintering (SPS) process. The results show that SPS method may realize the ultrafast crystallization of M-type barium ferrite, absolutely prevent the crystallization of intermediate phase α-Fe2O3, and significantly decrease the crystallization temperature of M-type barium ferrite. The sintered samples obtained at 800℃ by sintering the precursors for 10 minutes are a kind of multiphase ferrites composed of major phase M-type barium ferrite and trace amount of BaFe0.24Fe0.76O2.88. It is discovered that M-type barium ferrites in the holes of the sintered samples are in nanobelt microstructure about 100-300 nm in width and several micrometers in length. These M-type barium ferrite nanobelts are non-stoichiometric and may be expressed as BaFe12 xO19 1.5x (-4.77≤x≤6.50). Their composistions suggest completely random Fe-rich or Ba-rich domains.     

Near-infrared to visible up-conversion emissions of Er^3＋ doped Al2O3 powders derived from the sol-gel method

The Er3 doped Al2O3 powders were prepared by the sol-gel method using the aluminium isopropoxide [Al(OC3H7)3]-derived Al2O3 sols with addition of the erbium nitrate [Er(NO3)3.5H2O]. The different phase structure, including three crystalline types of (Al,Er)2O3 phases, γ, θ, α, and two Er-Al-O phases, ErAlO3 and Al10Er6O24, was obtained with the 1 mol% Er3 doped Al2O3 powders at the different sintering temperatures of 600―1200℃. The green and red up-conversion emissions centered at about 523, 545 and 660 nm, corresponding respectively to the 2H11/2, 4S3/2→4I15/2 and 4F9/2→4I15/2 transitions of Er3 , were detected by a 978 nm semiconductor laser diodes excitation. The phase structure and OH content had evident influence on the up-conversion emissions intensity. The maximum intensities of both the green and red emissions were obtained respectively for the Er3 doped Al2O3 powders sintered at 1200 ℃, which was composed mainly of α-(Al,Er)2O3, less of ErAlO3 and Al10Er6O24 phases, and with the least OH content. The two-photon absorption up-conversion process was involved in the green and red up-conversion emissions of the Er3 doped Al2O3 powders.     

Characterization of γ-Fe2O3 nanoparticles prepared by transfor- mation of α-FeOOH

γ-Fe2O3 nanoparticles were successfully synthesized by a chemically induced transformation of α-FeOOH.In this method,the precursor(α-FeOOH)was prepared by chemical precipitation,and then treated with a mixed FeCl2/NaOH solution to produce the nanoparticles.X-ray diffraction indicated that when the precursor was treated with FeCl2(0.22 mol/L)and NaOH(0.19 mol/L),pure γ-Fe2O3 nanoparticles were obtained.However,when the concentration of FeCl2 was<0.22 mol/L or the concentration of NaOH was<0.19 mol/L,α-FeOOH and γ-Fe2O3 phases co-existed in the nanoparticles.Transmission electron microscopy observations showed that in the samples with co-existing phases,the nanoparticles did not have identical morphologies.The pure γ-Fe2O3 nanoparticles were polygonal rather than spherical.The volume ratio of α-FeOOH and γ-Fe2O3 was estimated for the two-phase samples from magnetization data obtained from a vibrating sample magnetometer.This chemically induced transformation is novel,and could provide an effective route for the synthesis of other metal oxide nanocrystallites.     

Morphological characteristics of α-Al2O3 crystallites obtained direct1y from hydro /solvothermal solvents

The morphological characteristics of α-Al₂O₃ crystallites obtained directly from hydro/solv othermal solvents are reported and the formation mechanisms of corundum morphology are discussed from crystal growth and crystal chemistry principles. The crystal growth process is considered as a process of incorporation of growth units on the growth interfaces, and the crystal morphology is determined by the linkage of the coordinated polyhedra.     

Effects of aging on the microstructure of a Cu-Al-Ni-Mn shape memory alloy

The influence of aging on the microstructure and mechanical properties of Cu-11.6wt%Al-3.9wt%Ni-2.5wt%Mn shape memory alloy (SMA) was studied by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometer, and differential scanning calorimeter (DSC). Experimental results show that bainite, γ_2, and α phase precipitates occur with the aging effect in the alloy. After aging at 300dgC, the bainitic precipitates appear at the early stages of aging, while the precipitates of γ₂ phase are observed for a longer aging time. When the aging temperature increases, the bainite gradually evolves into γ₂ phase and equilibrium α phase (bcc) precipitates from the remaining parent phase. Thus, the bainite, γ₂, and α phases appear, while the martensite phase disappears progressively in the alloy. The bainitic precipitates decrease the reverse transformation temperature while the γ₂ phase precipitates increase these temperatures with a decrease of solute content in the retained parent phase. On the other hand, these precipitations cause an increasing in hardness of the alloy.     

Co-substituted ATS-type molecular sieves and films for cyclohexane oxidation

Pure CoAPO-36 crystal grains were synthesized by hydrothermal reaction. Porous α-Al₂O₃, stainless steel and K₂Ti₆O₁₃ supported CoAPO-36 films were fabricated using in situ crystallization for the first time. SEM images and XRD measurements demonstrate that a continuous CoAPO-36 film was obtained on the K₂Ti₆O₁₃ substrate. Diffuse reflectance UV-Vis spectra indicate that Co²⁺ has been incorporated into the ATS framework. Both CoAPO-36 crystal grains and the K₂Ti₆O₁₃ supported CoAPO-36 film exhibit satisfactory catalytic activities for the oxidation of cyclohexane.     

Synthesis of biodiesel from rapeseed oil using K2O/ γ -Al2O3 as nano-solid-base catalyst

Nano-solid-base catalyst K₂O/γ-Al₂O₃ was prepared and adopted for the synthesis of biodiesel by transesterification of rapeseed oil with methanol. The particle diameter of the catalyst was about 50 nm, which was measured by transmission electron microscopy (TEM). The variables affecting the yield of biodiesel during transesterification, such as mass ratio of KNO₃ to γ-Al₂O₃, calcination temperature, calcination time, and catalyst content, molar ratio of methanol to oil, reaction temperature and reaction time were investigated. The catalyst obtained by calcining a mixture of KNO₃ and γ-Al₂O₃ at 600 °C for 3 h, was found to be the optimum one, which gave the highest catalytic activity in reaction. With 3% (m _catalyst/m _oil) catalyst, when the transesterification carried out at a molar ratio of methanol to oil 12:1, a reaction temperature of 70 °C, and a reaction time of 3 h, yield of 94% was achieved. Foundation item: Supported by the National High-Technology Research and Development Program of China (863 Program) (2007AA100703)     

Dispersion of CoCl2 into γ-Al2O3 studied by positron

Co²⁺/γ-Al₂O₃ samples were prepared by incipient wetness impregnation of γ-Al₂O₃ with different concentration solution of CoCl₂ and dried at 40 °C. We measured the positron lifetime spectra of the samples of different Co²⁺ mass fractions (0%–8.24%) heated at different temperatures (100–500°C). All lifetime spectra were resolved into four components, in which the third and the fourth components were related to the surface state of the micropores and the secondary pores of the γ-Al₂O₃. The experimental results showed that the Co²⁺ was mainly located in the micropores and the secondary pores near to the exterior of the support. For low Co²⁺ mass fraction samples, when the heating temperature was above 400 °C, dispersal was almost finished. When the Co²⁺ mass fraction was above 5.59%, Co²⁺ and Cl⁻ were dispersed into the secondary pores in the form of multiple layers.     

Preparation and kinetics of the thermal decomposition of nanosized CuC2O4−ZnC2O4·2H2O

The physical mixture of nanosized CuC₂O₄−ZnC₂O₄·2H₂O, as precursors of CuO−ZnO, have been prepared by the one-step solid state reaction method at room temperature. The thermal decomposition processes taking place in the solid state oxalate mixture of nanometer CuC₂O₄−ZnC₂O₄·2H₂O have been studied in static air using TG, DSC, XRD and TEM techniques. TEM showed that the grain size of the decomposition product is 5–15 nm. The values of the activation energyE _α were determined using the isoconversional procedure of KAS method and the Ozawa method. The most possible mechanism functionf(α) of the thermal decompositions of nanosized CuC₂O₄−ZnC₂O₄·2H₂O are defined using the comparative method, function models of the decomposition of CuC₂O₄ and ZnC₂O₄ follow the same mechanism function “Avrami-Erofeev equation”. The pre-exponential factorA is obtained on the basis ofE _α andf(α), thus the thermal analysis kinetic triplet of the decompositions of nanosized CuC₂O₄−ZnC₂O₄·2H₂O are determined. Foundation item: Supported by the key Natural Science Fund of Deparartment of Science and Technology of Hubei Province (2001ABA099). Biography: CHEN Donghua(1946-), male, Professor, research direction: material synthesize and thermal, analysis kinetics.     

Structural phase transition in nanostructured γ-Fe_2O_3

Conclusions We have found that there is an exothermal peak on the DTA curve of nanostructured γ-Fe₂O₃ sample and that this peak is not repeatable. The XRD microstructure analysis confirms for the first time that this exothermal peak corresponds to the structural phase transition from γ-Fe₂O₃ to α-Fe₂O₃. After this transition, the nanostructured Fe₂O₃ crystalline grains grow continuously with increasing temperature.     

Manufacture of biomorphic Al2O3 ceramics using filter paper as template

Biomorphic Al₂O₃ ceramics were prepared through the surface sol-gel process with filter papers as bio-templates. The filter papers were infiltrated with γ-AlOOH sol and subsequently sintered in air at high temperatures to produce the biomorphic Al₂O₃ ceramics. The results show that the final materials have a hierarchical structure originated from the morphology of cellulose paper. The sintering temperatures exhibit a strong effect on the surface pore-size distribution of obtained Al₂O₃ ceramics. Differential scanning calorimeter, scanning electron microscopy, X-ray diffraction and BET analysis were employed to characterize the microstructure, morphology and phase compositions of the final products.     

超声波-化学沉淀法制备纳米氧化铝粒子

以硝酸铝和碳酸铵为原料,利用超声波与沉淀相结合的方法,制得了平均粒径为(12±2)nm的氧化铝超细粉末.反应生成的沉淀经XRD、TG和DTA实验分析知其化学组成为NH4Al(OH)2CO3,该沉淀在475K开始分解为氧化铝,在1273K几乎完全转化为θ-Al2O3.     

The comparative investigation on redox property and second-order nonlinear response of Keggin-type α-[PM12O39NPh]3− (M = W and Mo) and Mo6NPh

Keggin-type phenylimido-polyoxometalates α-[PM₁₂O₃₉NPh]³⁻ (M = W and Mo) have been systematically investigated on the electronic structures, redox as well as nonlinear optical (NLO) properties by density functional theory (DFT). The strong M≡N bond confirmed by natural bond orbital (NBO) analysis comprises one s bond and two π bonds, the same as Mo≡N in [Mo₆O₁₈NPh]²⁻. Furthermore, phenylimido segment effectively modifies the electronic properties of α-[PM₁₂O₃₉NPh]³⁻. On one hand, when enlarging the inorganic cluster from {Mo₆O₁₈} to {PMo₁₂O₃₉}, the energy gap between HOMO and LUMO in α-[PMo₁₂O₃₉NPh]³⁻ decreased, resulting in enormously anodic shift for the reduction potential, while the excitation energy is less and the total second-order polarizability β ₀ is up to 438-3×10⁻³⁰ esu, which is nearly 10 times larger than that of [Mo₆O₁₈NPh]²⁻. On the other hand, when metal W in α-[PM₁₂O₃₉NPh]³⁻ is substituted by Mo, the interaction between Mo and N is enhanced and the redox ability becomes stronger. The β ₀ value for α-[PMo₁₂O₃₉NPh]³⁻ is more than 5 times higher than that of α-[PW₁₂O₃₉NPh]³⁻. It indicates that changing appropriate metal or enlarging the inorganic cluster will improve the redox properties and second-order nonlinear response. Moreover, the electron transition for three compounds mentioned above occurred mainly from organoimido segment (as the electron donor) to polyanion cluster (as the acceptor). As a result, α-[PMo₁₂O₃₉NPh]³⁻ may be a promising candidate for oxidant and nonlinear optical material. Electronic Supplementary Material  Supplementary material is available for this article at and is accessible for authorized users. Supported by National Natural Science Foundation of China (Grant No. 20573016), Training Fund of NENU’s Scientific Innovation Project (Grant No. NENUSTC07017), Science Foundation for Young Teachers of Northeast Normal University (Grant No. 20070304) and Program for Changjiang Scholars and Innovative Research Team in University (PCSIRT)     

纳米Fe2O3-Al2O3复合材料的制备

采用溶胶-凝胶表面包覆法制备了纳米Fe₂O₃-Al₂ O₃复合材料, 利用X射线衍射和透射电镜对样品的物相、 粒度和形貌进行了研 究. 结果表明, α-Fe₂O₃掺杂降低了Al₂O₃相变温度, 在900 ℃可以得到稳定的α-Al₂O₃相.     

Fast formation of NaA zeolite membrane in the microwave field

NaA zeolite membrane was successfully synthesized on the porous α-Al₂O₃ support by microwave heating. The synthesis of NaA zeolite membrane in the microwave field only needs 15 min and the synthesis time is 10 times shorter than that by conventional heating. SEM characterization indicates that the zeolite crystals in the NaA zeolite membrane synthesized by microwave heating are uniform in size; the membrane thickness is about 4 μm and is thinner than that of the NaA zeolite membrane synthesized by conventional heating. Gas permeation studies indicate that the permeances of the NaA zeolite membrane synthesized by microwave heating are 3–4 times higher than those of the NaA zeolite membrane synthesized by conventional heating, while their permselectivities are comparable.     

Syntheses and lyotropic liquid crystal properties of a series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30

A series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30, Na16[As4W30M4(H2O)2O112]·XH2O (M = Zn,Cu,Co,Ni,Mn and Cd), have been synthesized for the first time and structurally characterized by elemental analysis, IR and 183W NMR spectra. The crystal structure of Na16[As4W30Cu4(H2O)2O112]·63H2O was determined to be a triclinic system, of P1 symmetry, a = 1.2721(3) nm, b = 2.451 6(5) nm, c = 2.6450(5) nm, α= 89.90(3)°,β= 77.32(3)°, γ= 89.96(3)°, 2=2. Using tetrahepty lammonium bromide as a phase transfer reagent, [As4W30Cu4(H2O)2O112]16- was transferred from aqueous solution to organic phase (benzene), and the heteropolyanion lost the coordination water molecules to form the coordination-unsaturated ion. After lactic acid was added to the benzene solution, the coordination-saturation was recovered. By esterification reaction between lactic acid and cholesterin, the latter was attached to the heteropolyanion indirectly. Therefore, a new type of lyotropic liquid crystal was obtained, which was characterized by a polarimicroscope, DSC and variable temperature wide-angle X-ray diffraction.     

单极性脉冲电流密度对铝合金MAO膜相结构和微结构的影响

利用微弧氧化(MAO)技术在铝合金表面沉积陶瓷膜, 采用X射线衍射仪(XRD), 扫描电子显微镜(SEM), 电子能谱(EDS)和显微硬度方法, 研究了MAO过程中单极性脉冲电流密度与氧化膜力学性能和化学成分的关系. 发现在较高电流密度下制备的陶瓷膜中含有较多的α-Al₂O₃相, 而在较低电流密度下制备的陶瓷膜主要由γ-Al₂O₃相组成. 对陶瓷膜截面上不同厚度处的膜层化学成分分析表明, 组成氧化膜的主要物质α-Al₂O₃和γ-Al₂O₃的比例随深度的变化呈现出复杂的变化规律, 这一结果与相关的文献报道有所不同.