Synthesis of polycrystalline alumina fibre with aluminium chelate precursor

Polycrystalline alumina fibre was successfully synthesized by pyrolysis of preceramic fibre formed from aluminium chelate compound. Ethyl 3-oxobutanoatodiisopropoxyaluminium (EOPA) was reacted with glacial acetic acid yielding a polymeric product. The absorption bands ascribed to Al-O from 630–705 cm^–1 changed from a sharp to a broad band on treatment with acetic acid. The¹³CNMR spectrum of EOPA changed from sharp singlets to multiplets after the reaction with acetic acid. The viscosity of the polymeric product increased in intensity with increasing amount of acetic acid. The viscosity of the polymeric product formed from EOPA-30 mol % acetic acid was 450 Pa s at 30 °C, and decreased to 5.4 Pa s with increasing measurement temperature from 30–70 °C. The²⁷Al resonance at 35 p.p.m. increased in intensity with increasing viscosity of the polymeric precursor. The molecular weight of the precursor was distributed from 400–800. The polymeric precursor pyrolysed at 500 °C in air was amorphous to X-rays, and crystallized in -alumina at 840 °C. The precursor fibres were pyrolysed, to yield fine-grained fibres of -alumina, at 1300 °C for 1 h.     

The formation of β′-sialon from a montmorillonite-polyacrylonitrile composite by carbothermal reduction: an NMR,TGA, XRD and EM study

The products of carbothermal reduction in N₂ of a nanocomposite between dodecylammonium-exchanged montmorillonite and polyacrylonitrile (PAN) have been studied by solid-state ²⁷Al and ²⁹SiNMR spectroscopy, X-ray diffraction, transmission electron microscopy and thermogravimetry. Comparison with analogous reactions involving sodium-exchanged montmorillonite and dodecylammonium-exchanged montmorillonite (without PAN) shows that in the presence of PAN, the formation of silica, cordierite or mullite is almost completely suppressed. The only crystalline phase detected between 1000 and 1300 °C was a -sialon, having a much higher SiAl ratio (7.051) than that of the precursor clay (2.441). Reduction of the octahedral AlO₆ begins near 1200 °C, forming increasing amounts of Al(N,O)₄ tetrahedra with temperature, so that by 1600 °C, complete reduction to AlN₄ (i.e. bulk AlN) has occurred. In contrast, reduction of the tetrahedral SiO₄ is appreciable at 1100 °C, and is almost complete (SiN₄ tetrahedra only) by 1200 °C. No intermediate Si(N,0)₄ environments are found. By 1600 °C, only the SiC₄ environment (i.e. bulk SiC) remains. A mechanism is suggested, involving the formation of alternating slabs of an amorphous aluminosilicate and carbon at 1000 °C, followed by diffusion of silicon from the outer regions of the aluminosilicate band towards the centre, and sequential reduction of Si(OSi)₄ and Si(OSi)₃ (OAl) groups.     

Structure of nickel-doped α-FeOOH

Colloidal particles of nickel-doped-FeOOH prepared under varied conditions were characterized using transmission electron microscopy, X-ray diffraction thermogravimetry-differential thermal analysis, Fourier transform infrared analysis, inductively coupled plasma spectroscopy and nitrogen adsorption. The unit cell dimensions of the resulting-FeOOH slightly changed on doping with nickel. Both the total and surface hydroxyl ions decreased with increasing amounts of nickel. The nickel content in the surface layer determined by X-ray photoelectron spectroscopy was larger than the total nickel content determined by inductively coupled plasma spectroscopy. The results obtained indicate that the substitution of iron with nickel took place in the surface layer more than in the internal phase.     

Self-Diffusion of Iron in Molten Fe-C Alloys

Self-diffusion coefficients of iron in molten Fe-C alloys have been measured by using the capillary method. In addition, the samples have been autoradiographed and sectioned to insure that no significant convection has occurred during the diffusion. The results can be represented by the equation D = 4.3×10^?3 exp (—12.200/RT) for carbon = 4.6 pct and T = 1513° to 1633°K; and D = 1.0×10^?2 exp (—15,700/RT) for carbon = 2.5 pct and T = 1613° to 1673°K. The D values are higher and the heat of activation for diffusion lower in alloys containing more carbon. Calculation based on the Einstein-Stokes equation indicates that the diffusing species is iron ion.     

Reaction sintering of Fe-Al-Si alloys

The present study concerns the production of multiphase alloys of the Fe-Al-Si system using a powder metallurgical approach. Several compositions have been considered based on α-Fe, α′-FeAl; and α″-Fe₃Al intermetallic phases. Elemental powder mixtures were compacted and sintered in a dilatometer. In this way, the dimensional changes involved with thermally induced transformations could be followed during continuous heating runs up to the sintering temperature. The effect of heating rate has been considered. The characterization of the final products was based mainly on x-ray diffraction (XRD) analyses, particularly as concerns the quantification of the crystalline phases present in the final products. Grain and porosity morphologies were characterized by scanning electron microscopy (SEM). In this way, clear indications of the reaction and densification processes occurring during the sintering treatments were obtained.     

Influence of Atomizing Gases on the Oxide-Film Morphology and Thickness of Aluminum Powders

Fine powders of aluminum were produced in a pilot-plant, inert-gas atomizerwith a confined-design nozzle, which operated vertically upward. Argonand helium at 1.85 MPa and nitrogen at 1.56 MPa were used as the atomizingagent. The morphology of the powder particles was examined by SEM. Powderswere sieved dry and wet. The Sauter mean diameter of the powders varied from20.70 to 10.25 m depending on the atomizing gas. The distribution ofsizes was bimodal. The mean thickness of oxide on the surface of the powderwas calculated from the total oxygen contents of powder samples (determinedby a Leco analyzer). In addition, ESCA measurements and BET tests werecarried out for surface-oxide thickness and area measurements,respectively. The finest powder produced under helium incorporated thinnersurface-oxide layers than the coarser ones produced under argon andnitrogen. This was due to differences in physical properties (such asdensity, thermal conductivity) and flow properties (such as gasvelocity and relative velocity) of the atomizing gases used, i.e., helium,argon, and nitrogen. The oxide was very irregular in thickness in thecoarse-size range of the Al powders produced under argon and nitrogen. Thiswas presumably because of the high- and low-temperature oxidation ofaluminum droplets during the atomization and subsequent solidification andcooling periods leading to the rough surfaces observed with SEMinvestigation in the present work.     

Size and pressure effects on solid transition temperatures of ZrO2

Transition temperatures between tetragonal and monoclinic polymorphs of ZrO₂ nanoparticles, thin films and nanostructured materials are calculated by considering energetic contributions of surface (interface) energy and surface stress on total Gibbs free energy. The transition temperatures drop as the size of the nanocrystals decreases, which is consistent with available results.     

Sensing tool breakage in face milling with a neural network

A new approach using a neural network to process the features of the cutting force signal for the recognition of tool breakage in face milling is proposed. The cutting force signal is first compressed by averaging the cutting force signal per tooth. Then, the average cutting force signal is passed through a median filter to extract the features of the cutting force signal due to tool breakage. With the back propagation training process, the neural network memorizes the feature difference of the cutting force signal between with and without tool breakage. As a result, the neural network can be used to classify the cutting force signal with or without tool breakage. Experiments show this new approach can sense tool breakage in a wide range of face milling operations.