Constitutive modeling of deformation in high temperature of a forging 6005A aluminum alloy

The 6005A aluminum alloy is one of the most widely used alloys in aeronautic and railway industries, yet its plastic deformation behavior under hot compression is still not fully understood. Isothermal compression tests of 6005A aluminum alloy were performed using a Gleeble-1500 device, up to a 70% height reduction of the sample at strain rates ranging from 0.01 s⁻¹ to 10 s⁻¹, and deformation temperatures ranging from 573 K to 773 K. Several modeling approaches, including flow stress–strain curves, a constitutive Arrhenius-type equation model, and processing maps were used to characterize the deformation behavior of the isothermal compression of 6005A aluminum alloy in this study. The related material constants (i.e. A, β and α) as well as the activation energy Q for 623–773 K and 573–623 K temperature regimes were determined. Two sets of constitutive exponent-type equations for the 6005A aluminum alloy were proposed. Furthermore, a change in deformation mechanism occurred when changing the temperature range from 623–773 K to 573–623 K.     

Study on the flash pyrolysis of polyacrylamide: accelerator of Al–H<Subscript>2</Subscript>O-based propellants

The flash pyrolysis of polyacrylamide (PAM) in Ar atmosphere was carried out in a tube-type pyrolyzer at 700 °C for 5 min. The volatile products were detected and identified by gas chromatography combined with mass spectrometry (GC/MS). Twenty four kinds of pyrolysis products were identified. In particular, some products, such as acetaldazine and 4-hydroxy-4-methyl-2-pentanone, were the first reported existing in the PAM pyrolysis products, which should play an important role in improving the igniting and combustion performance of Al–H₂O-based propellants. Moreover, the flash pyrolysis residues were analyzed by FTIR. The experimental results show that the pyrolysis products of PAM can be roughly divided into five types. The products of five types promote the igniting and combustion performance of Al–H₂O-based propellants, and the mechanisms of formation of every type are discussed.     

High-temperature study of zirconia gels: Evolution of surface area and porosity on calcination in a vacuum

Zirconium dioxide, prepared by dehydration of a zirconia gel, was calcined in a vacuum at temperatures ranging from 573 to 1173K, in order to investigate the evolution of specific surface area and porosity as a function of the calcination temperature. The results are compared with those previously obtained for samples heated in air.Samples fired up to 773 K were found to be basically microporous, with surface areas ranging from 142 to 93 m²g^?1. Calcination at 973 K led to total elimination of microporosity and reduction of surface area by about 50%. In the temperature range 773–1173 K, the most frequent pore radius was found to increase from 1.5 to 10.5 nm as the temperature was raised.     

Pyrolysis treatment of oil sludge and model-free kinetics analysis

Pyrolysis of tank bottom oil sludge was investigated to summarize the pyrolysis characteristics through analyzing the change of mass loss, pyrolysis gas compositions in heating process. For this propose, various approaches including thermogravimetric analysis (TGA), CNHS/O elemental analysis, electrically heated fixed bed quartz reactor coupled with Vario Plus emission monitoring system, and oil-gas evaluation workstation (OGE-II) equipped with a flame ionization detector (FID) were used. The pyrolysis reaction is significant in the range of 473-773 K where multi-peak DTG curves can be gained. Higher heating rate increases the carbon (C) and sulfur (S) contents but decreases hydrogen (H) content in solid residues. The major gaseous products excluding N(2) are CHs (Hydrocarbons), CO(2), H(2), CO. The yield of CHs is significant in the range of 600-723 K. Higher heating rate causes the peak intensity of CHs evolution to increase and the CHs evolution to move towards a high-temperature region. Around 80% of total organic carbon content (TOC) in oil sludge can be converted into CHs in pyrolysis process. The CHs data were used for kinetic analysis by Vyazovkin model-free iso-conversion approach. Dependences of the activation energy on the degree of conversion obtained from different methods were compared.     

Synthesis of a minute SiC product from polyvinylsilane with radiation curing: Part II—Ceramization process of radiation cured polyvinylsilane

We have synthesized minute SiC products from polyvinylsilane (PVS), which is a liquid organosilicon polymer, with radiation curing. Since there is a close relationship between the properties of obtained SiC products and pyrolysis condition, it is important to investigate the ceramization process of cured PVS in order to find out the optimum pyrolysis condition. In this paper, the ceramization process of the PVS cured by γ-ray irradiation at room temperature was investigated by gas analysis, thermogravimetric analysis (TGA), density measurement, and so on. It was found that the ceramization of γ-ray cured PVS starts above 500 K, and drastic organic–inorganic conversion occurs in the temperature range of 700–1100 K. According to the changes of mass and density, it was found that the volume shrinkage of PVS during the curing and pyrolysis processes is 80%. The SiC obtained by pyrolysis at 1573 K in argon gas atmosphere showed the density of 2500 kg/m³ and microvickers hardness of 31.6 GPa.     

Phase-transition studies on copper ferrite

Electrical resistivity of nominal CuFe₂O₄ subjected to various thermal pretreatments was measured in air and argon at different temperatures between 373 and 773K. The log ρ → 1/T plots obtained while heating and cooling the slowly cooled tetragonal sample in air showed a hysteresis loop in the range 533–693K due to a first-order diffusionless and reversible phase-transition. The corresponding plots for cubic CuFe₂O₄, quenched from 1173K, showed the phase-transition to be irreversible and accompanied with diffusion of ions. Samples quenched from intermediate temperatures between 783 and 1173K were metastable tetragonal spinels, undergoing an irreversible phase-transition accompanied by ionic diffusion. The extent of diffusion in these samples was found to be dependent on the quenching temperature decreasing with increasing temperature.     

Pyrolysis temperature and time dependence of electrical conductivity evolution for electrostatically generated carbon nanofibers

Carbon nanofibers were produced from polyacrylonitrile/N, N-Dimethyl Formamide (PAN/DMF) precursor solution using electrospinning and vacuum pyrolysis at temperatures from 773-1273 K for 0.5, 2, and 5 h, respectively. Their conductance was determined from I-V curves. The length and cross-section area of the nanofibers were evaluated using optical microscope and scanning probe microscopes, respectively, and were used for their electrical conductivity calculation. It was found that the conductivity increases sharply with the pyrolysis temperature, and increases considerably with pyrolysis time at the lower pyrolysis temperatures of 873, 973, and 1073 K, but varies, less obviously, with pyrolysis time at the higher pyrolysis temperatures of 1173 and 1273 K. This dependence was attributed to the thermally activated transformation of disordered to graphitic carbon.     

Construction and Verification of the Constitutive Model of Pure Copper Deformation at Elevated Temperatures

Strength of Materials - The deformation behavior of pure copper was studied in hot compression tests in the temperature range of 773–1173 K and strain rate interval of 0.001–1.0...     

Effect of surface treatment on segregation of impurities in haematite

Surface segregation of various impurities such as Mg, Si, Ca, Al and Cr were determined for the haematite phase (Fe₂O₃) annealed in two different gas compositions involving (1) air at 1173 K, and (2) a gas mixture containing sulphur at 773 K. The objective of work was to establish the effect of the gas-phase composition on segregation of lattice defects. The near-surface segregation profiles of the impurities were determined by secondary ion mass spectrometry. The depth profile analysis was made by sputtering using an Ar⁺ primary beam of energy 30 keV. The surface charge was neutralized by an electron gun. It was found that annealing Fe₂O₃ under a gas phase containing sulphur resulted in the formation of an Fe(SO₄)₃ surface layer. It was observed that the two surface treatment procedures applied (both with and without sulphur) result in Mg enrichment in the near-surface region of Fe₂O₃. Si and Ca exhibit an enrichment and impoverishment after the surface treatments 1 and 2, respectively. Finally, the near-surface layer is impoverished in Cr and Al after both types of surface treatment. Experimental results are discussed in terms of segregation driving forces of the respective elements and the possible effect of sulphur on the gas-solid heterogeneous kinetics.     

Effect of sintering temperature on the properties of Cu-Co ferrites prepared by oxalate precipitation method

Polycrystalline Cu-Co ferrite powder was synthesized following oxalate precipitation method. The samples of the compound Cu_0.5Co_0.5Fe₂O₄ were heated at different temperatures in the range of 773-1173 K and were characterized by X-ray diffraction and SEM techniques. The results of XRD show the formation of single-phase cubic spinel structure. The lattice parameter showed a minimum value for the sample heated at 1073 K. It has been observed that grain size increases with the increase in temperature and is maximum (3.2 μm) for the powder sintered at 1173 K.     

Phase evolution and reaction mechanism during reduction–nitridation process of titanium dioxide with ammonia

Titanium nitride powders were synthesized from titanium dioxide at 1173–1373 K in ammonia atmosphere. The reduction–nitridation products with various fractions obtained at various temperatures were analyzed by X-ray diffraction, Raman spectra, X-ray photoelectron spectroscopy, scanning electron microscope, transmission electron microscopy, and selected area electron diffraction. The reaction sequence from TiO₂ to TiN in ammonia atmosphere was changed by increasing the reaction temperature. The reaction sequence at 1173 K was found as TiO₂ → TiN_1?xO_x → TiN. When the reaction temperature was above 1273 K, the reaction sequence changed to as follows: TiO₂ → Ti₉O₁₇ → TiN_1?xO_x → TiN. Ti₃O₅ was not found as an intermediate phase on account of its instability in NH₃ atmosphere. The morphology of the synthesized TiN is closely related to that of the raw materials.     

Estimation of the heat required for intermediate pyrolysis of biomass

Biomass waste contains an abundant source of energy that can be transformed into high-calorific fuel during intermediate pyrolysis, consequently reducing the use of fossil fuel resources. In the present study, medium density fibreboard (MDF), brewery spent grains (BSG) and post-extraction soybean meal (SM) were used to pyrolysis. Valorisation of these wastes via intermediate pyrolysis was carried out at a temperature of 773 K in a fixed-bed reactor under nitrogen atmosphere. The ultimate analysis showed that MDF char has offered the highest carbon content. Generally, chars obtained from these feedstocks were characterized by different internal microstructures. On the one hand, the surface of MDF char has exhibited pores with a regular pattern of small perpendicular blocks. On the other hand, irregular open spaces were detected in BSG and SM chars. The results of this investigation of the microstructure proved that the studied biomass wastes are perspective feedstocks to obtain high-value bioenergy products. Based on the enthalpy balance, it was concluded that the heating value of the pyrolysis gas was higher, the more endothermic pyrolysis process. The research hypothesis confirms that the higher the K₂O/CaO ratio in the ash, the better biomass pyrolysis process was catalysed and as a result, less additional heat was required for pyrolysis. To carry out the pyrolysis of MDF, SM and BSG, additional heat input was required in the amount of 2016.8, 1467.9 and 881.1 kJ, respectively. It was found that 4–10% of the higher heating value of the raw materials was missing to achieve the self-sustaining energy of intermediate pyrolysis.

Graphical abstract

     

Modification of the properties of tin sulfide films grown by spray pyrolysis

n-Type SnS and SnS₂ sulfide films up to 0.6 μm in thickness, with resistivity in the range 2 ≤ ρ ≤ 17 kΩ cm have been grown by spray pyrolysis of aqueous solutions of the SnCl2 ? 2H₂O, SnCl₄ ? 5H₂O, and (NH₂)₂CS salts at substrate temperatures in the range 523 ≤ T_s ≤ 623 K. At constant thermal conditions of sulfide film growth, varying the chemical composition of the solutions for spray pyrolysis makes it possible to obtain films with substantially different optical properties. Undoped SnS and SnS₂ have high transmittance, T ≈ 40–70%, and a sharp intrinsic absorption edge. The optical band gap of the SnS and SnS₂ sulfide films has been shown to depend on film growth conditions.     

Alloying behaviour,thermal stability and phase evolution in quinary AlCoCrFeNi high entropy alloy

An equiatomic quinary AlCoCrFeNi high entropy alloy (HEA) has been synthesized by mechanical alloying. Milled powder after 30?h shows good chemical homogeneity and refined morphology with a mean particle size of ～4?μm. Solid solution phase with BCC crystal structure (a?=?2.89?±?0.02?Å) has been confirmed from XRD and transmission electron microscopy in the as-synthesized high entropy alloy. The milled alloy powder is not thermally stable. Differential scanning calorimetric (DSC) thermogram of 30?h milled powder exhibits the presence of a small peak at ～600?°C (873?K) with a thermal shift near the peak. This thermal shift indicates the diffusive type of phase transformation in this alloy while heating. The analysis of the in-situ heating X-ray diffraction patterns at various temperatures extends support to the diffusive nature of the phase transformation. Upon heat treatment, the disordered BCC solid solution phase partially transforms to Ni₃Al prototype L1₂ phase which precipitates at a lower temperature (350?°C (623?K)) as observed by in-situ XRD experiments. However, at high temperature annealing (575–800?°C (848–1073?K)) the evolution of a partially ordered BCC phase (B2) with lattice parameter (a?=?2.87?±?0.02?Å), and L1₂ phase (a?=?3.58?±?0.05?Å), along with tetragonal σ phase (a?=?8.8?Å and c?=?4.53?Å) are observed. Similar types of phases have also been identified after annealing and microwave sintering at 800?°C (1073?K) & 900?°C (1173?K) respectively. The transformation of ordered BCC phases along with two intermetallics such as L1₂ phase and σ phase suggests that the evolution of the high entropy phase in the milled condition leads to a combination of high entropy and medium entropy phases in the annealed condition.     

Application of pyrolysis–gas chromatography/mass spectrometry for the identification of polymeric materials in failure analysis in the automotive industry

The application of analytical pyrolysis–gas chromatography mass spectrometry (Py–GC/MS) in the failure analysis of two hydraulic cylinders and their rubber membranes from the automotive industry were presented.     

Microstructure, martensitic transformation and superelasticity of Ti49.6Ni45.1Cu5Cr0.3 shape memory alloy

The aim of this study is to investigate the microstructure, martensitic transformation behavior, shape memory effect and superelastic property of Ti_49.6Ni_45.1Cu₅Cr_0.3 alloy, with Cu and Cr substituting for Ni. After annealing, the alloy showed single step A-M/M-A transformations within the whole annealing temperature range of 623 K to 1273 K even in the presence and Ti₂(Ni, Cu) precipitates. With the increase of the annealing temperature, the transformation temperatures exhibited three stages: increasing from 623 K to 873 K, decreasing from 873 K to 1023 K and unchanging from 1023 K to 1273 K. Meanwhile, the critical stress for stress induced martensitic (SIM) transformation decreased to a minimum value and increased after that, exhibiting a V shape curve. The alloy annealed at 623, 773 and 923 K exhibited shape recovery ratio more than 90% when the deformation strain was below 20%.     

全氟己酮灭火剂高温热裂解性能研究

基于GC、GC-MS和KM900手持式烟气分析仪测试手段,研究了全氟己酮在管式反应器中滞留时间为2s和5 s、裂解温度为500~750℃时的热裂解规律。结果表明:全氟己酮在550℃时开始分解,超过650℃裂解剧烈;主要裂解气体产物为十氟丁烷、六氟丙烯和全氟异戊烷;随着裂解温度和滞留时间的增加,全氟己酮裂解程度加剧,十氟丁烷和六氟丙烯生成量增加,全氟异戊烷的生成量先增加后减少;值得重视的是全氟己酮高温热裂解时有剧毒气体全氟异丁烯和毒性气体一氧化碳产生。     

Structural stability and mechanochemical activity of titanium nitride prepared by mechanical alloying

Pure titanium nitride (TiN) was synthesized by mechanical alloying (MA). In order to prevent the contamination from the MA vial and atmospheric gas, the MA steel vial was replaced with a titanium vial and atmospheric gas was deoxidized using sponge titanium heated to 623 K. The mechanochemical activity during MA was estimated from the gas purification temperature. The investigation of thermal and pressure stability by thermal treatment and hot isostatic pressing (HIP) revealed that titanium nitride, TiN, was stable on heating to 1173 K under a vacuum, but became unstable under a high pressure, 100 MPa.     

Quasicrystal–crystal structural transformation in Al–5 wt.% Mn alloy

The atomic structure of Al–5 wt.%Mn (Al–5Mn) alloy, prepared by rapid solidification, and pre-annealed at 623 and 773 K for 5 and 1 h, respectively, were characterized by X-ray powder diffraction (XRD) and extended X-ray absorption fine structure (XAFS) techniques. The sample in as-quenched stage was found crystalline, consisting of metastable α-Al (Al–Mn solid solution) and icosahedral quasicrystalline I-Al₆Mn phases. Five hours annealing at 623 K proved thermal stability of both the phases. Pre-annealing at 773 K/1 h on the other hand leads to α-Al phase decomposition and structural transformation of metastable I-Al₆Mn to stable orthorhombic Al₆Mn phase. The EXAFS results indicate that Mn atoms are located preferably on the outer shell of icosahedrons. During the I-Al₆Mn→o-Al₆Mn transformation the total Al atoms coordinating one Mn were found to be constant (∼10). Based on the results, only distance/symmetry changes in atomic arrangement around Mn atoms were suggested.     

Application of gas chromatography/mass spectrometry (GC/MS) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) in failure analysis in the automotive industry

This paper describes the application examples of gas chromatography/mass spectrometry (GC/MS) and pyrolysis–gas chromatography/mass spectrometry (Py-GC/MS) in failure analysis for the identification of chemical materials like mineral oil from a malfunctioning motorbike and a complaint car tire rubber. Furthermore, failure case demanding identification of chemical composition of solid plastic particles from a failed mechanical engineering component is demonstrated. The obtained analytical results were then used for troubleshooting and remedial action of the technological processes.