Modeling of hot isostatic pressing of metal powder with temperature–dependent cap plasticity model

In this paper, the coupled thermo–mechanical simulation of hot isostatic pressing (HIPing) is presented for metal powders during densification process. The densification of powder is assumed to occur due to plastic hardening of metal particles. The constitutive model developed is used to describe the nonlinear behavior of metal powder. The numerical modeling of hot powder compaction simulation is performed based on the large deformation formulation, powder plasticity behavior, and frictional contact algorithm. A Lagrangian finite element formulation is employed for the large powder deformations. A modified cap plasticity model considering temperature effects is used in numerical simulation of nonlinear powder behavior. The influence of powder-tool friction is simulated by the use of penalty approach in which a plasticity theory of friction is incorporated to model sliding resistance at the powder-tool interface. Finally, numerical examples are analyzed to demonstrate the feasibility of the proposed thermo–mechanical simulation using the modified cap plasticity model in the hot isostatic forming process of powder compaction.     

Effect of hot isostatic pressing on mechanical properties and microstructure of 70–30 cupronickel castings

Abstract

The present work is part of an investigation into the use of hot isostatic pressing to recover 70–30 cupronickel castings. These alloys have particularly good corrosion resistance and, when strengthened with silicon and chromium, produce a material capable of use in very severe conditions of stress and massive corrosion. However, it is not possible to recover such castings by the application of repair welding, because of the possibility of reduced corrosion resistance in the vicinity of the weld. Hot isostatic pressing represents an alternative method of casting recovery. The results reported in the present work refer to the effect of hot isostatic pressing on mechanical properties, microstructure, and the level of segregation in the alloys. Hot isostatic pressing may be used to remove casting defects in the form of fine pores up to total porosity of 5%. However, in cases where porosity takes the form of very large defects, the mechanical properties of the recovered region are inferior to those of the originally sound material. This effect is probably associated with the presence of very finely distributed oxide particles in the originally defective parts of the casting. The optimum hot isostatic pressing temperature for the best overall combination of properties was 950°C.

MST/1732     

Mechanical and thermal expansion properties of β-eucryptite prepared by sol–gel methods and hot pressing

The microstructures, mechanical properties and thermal expansion behavior of monolithic lithium aluminosilicate glass–ceramics, prepared by sol–gel method and hot pressing, were investigated by using X-ray diffraction, scanning and transmission electron microscopies, three-point bend tests and dilatometry. β-eucryptite appeared as main phase in the monolithic lithium aluminosilicate glass–ceramics. The glass ceramics exhibited high relative densities and the average flexural strength and fracture toughness values were 154 MPa and 2.46 MPa m^1/2, respectively. The lithium aluminosilicate glass–ceramics hot pressed 1300 and 1350 °C demonstrated negative coefficient of thermal expansion, which was affected by amount and type of crystalline phases.     

Self-reinforcement in li-α-sialon ceramics

Self-reinforcement of Li--sialon ceramics by in situ growth of elongated and -sialon grains has been explored and analysed. Properties of Li--sialon ceramics are mainly determined by the overall starting composition and the crystalline modification of the starting Si₃N₄ powder which in turn determine the final microstructure of the materials. Both the morphology and crystalline phase of the elongated sialon grains have strong effects on the toughening mechanism. The results indicate that -sialons reinforced by elongated -sialon grains have advantages over similar materials reinforced by elongated -sialon grains because of the type of crack deflection toughening mechanism involved.     

Densification process of α′-sialon ceramics

The liquid-phase sintering process of -sialon ceramics has been investigated by high-temperature dilatometry and microstructural observation. In addition, isothermal shrinkage measurements have been performed to examine the densification kinetic parameter. It has been confirmed that densification kinetic parameters in the solution-reprecipitation stage are much larger than the rate exponent predicted for the classic liquid-phase sintering model, and are slightly smaller than that for the viscous flow process. Rapid shrinkage was observed in the solution-reprecipitation stage from the results of shrinkage rate, and corresponds to pore elimination by particle rearrangement and cooperative flow of particle/liquid mixture. These processes provide the major contribution to shrinkage. In addition, the liquid flow process occurs when the silica content in the raw powder increases, but it is retarded due to the formation of -sialon. It is anticipated that particle rearrangement and cooperative flow, as well as liquid-flow processes, take place in the solution-reprecipitation stage of sintering of Si₃N₄-based materials, and cause a large amount of shrinkage.     

A study on preparation of Mo–0.6Ti–0.2Zr–0.02C alloy by mechanical alloying and hot isostatic pressing,and its characterization

Mo–0.6Ti–0.2Zr–0.1C alloy was prepared by mechanical alloying (MA) and subsequently consolidated by powder processing techniques. The pellets prepared from the fine size MA powder showed a high rate of densification during sintering in the temperature range of 1300–1500 °C. Close to theoretical density was attained by hot isostatic pressing (HIP) at 1250 °C and TEM studies revealed the uniform distribution of complex carbide precipitates (<100 nm) in the fine grain microstructure of the consolidated alloy. The alloy consolidated by HIP showed a high hardness of the order of 500 HK due to the presence of the carbides in the fine grain microstructure.     

Effect of processing on toughness of Ca α-sialon ceramics

The influence of processing on microstructural development of Ca -sialon composition (Ca _x Si_12–3x Al_3x O _x N_16–x ) with x = 1.8 was studied by dwelling at different intermediate temperatures before reaching the final sintering temperature. The microstructural observation results have showed the different aspect ratios of elongated grains obtained by the various processing conditions, reflecting the effect of the number of nuclei of -sialon on morphology of grains during sintering. Improved toughness was achieved by applying low temperature dwelling for Ca -sialon compositions with low x values. The toughness showed an increase of 33% and 16% for x = 0.6 and 1.0 compositions respectively with middle dwelling processing at 1350°C for 3 h before reaching 1750°C for 1 h by hot-pressing.     

Mechanical properties of nanostructured Al2024–MWCNT composite prepared by optimized mechanical milling and hot pressing methods

Nanostructured Al2024–multiwall carbon nanotubes (MWCNTs) composites were produced using optimized mechanical milling and hot pressing methods. Nanostructured Al2024 powder was first prepared through 30 h mechanical milling of the alloy powder. MWCNTs up to 3 vol.% were added to the milled Al2024 powder and milled for different times. Differential thermal analysis (DTA) and X-ray diffraction (XRD) were used to assess the structural changes and thermal behavior during mechanical milling and hot pressing. Hardness and compression tests were applied on bulk samples to evaluate their mechanical properties. Mechanical milling applied on Al2024 powders for 30 h resulted in the grain refinement to ～30 nm. DTA analysis showed an endothermic peak at ～632 °C due to Al2024 melting and an exothermic peak between 645 and 658 °C related to Al and MWCNTs reaction. Mechanical milling of nanocomposite powder for 4 h and following hot pressing at 500 °C under a pressure of 250 MPa for 0.5 h were selected as optimized conditions for bulk nanocomposite preparation. With MWCNTs addition up to 2 vol.%, relative density remained at 98%, and hardness increased to 245 HV. Compressive strength of nanocomposites found a maximum value of 810 MPa at 2 vol.% MWCNTs addition which is 78%, 34% and 12% greater than that for Al2024–O, Al2024–T6 and nanostructured Al2024, respectively.     

Dense polycrystalline β-tricalcium phosphate for prosthetic applications

A method is described for preparing dense, polycrystalline-tricalcium phosphate. The compressive and flexural strengths of the polycrystalline bodies sintered at a temperature of 1150° C for 1 h were found to be 459 and 138 MPa, respectively. Observation of the fracture surfaces by scanning electron microscopy indicates a predomination of transgranular failures. The polycrystalline tricalcium phosphate is non-toxic in a cell culture system.     

Novel sponge-like structure created in GdBa2Cu3O7−δ ceramics by hot spot

A hot spot, which is a local area glowing orange, appears in a GdBa₂Cu₃O_7−δ ceramic rod when a voltage exceeding a certain value is applied to the rod at room temperature. The rod with the hot spot shows various functional characteristics that give rise to applications in devices. We found that the hot spot created a sponge-like structure in the rod. The elemental map revealed that the sponge-like structure was composed of Gd₂BaCuO₅ grains. The hot spot is considered to decompose GdBa₂Cu₃O_7−δ into Gd₂BaCuO₅ and liquid phase, and the liquid phase moves toward the periphery of the rod, leaving sponge-like structure composed of Gd₂BaCuO₅ grains. The novel sponge-like structure created in the GdBa₂Cu₃O_7−δ rod by the hot spot may bring about new applications for magnetic separations of fluids.     

Densification and Microstructure of β-sialon/Nano-size SiC Composites

β-sialon/nano-size SiC composite ceramic with DyAG(Dy3Al5O12) as grain boundary phase was fabricated through hot-pressing. The effect of nano-size SiC on densification, phase composition, microstructure and mechanical properties of the materials was studied     

Tribological properties of Al6061–Al2O3 nanocomposite prepared by milling and hot pressing

Tribological properties of bulk Al6061–Al₂O₃ nanocomposite prepared by mechanical milling and hot pressing were investigated. Al6061 chips were milled for 30 h to achieve a homogenous nanostructured powder. A 3 vol.% Al₂O₃ nanoparticles (∼30 nm) were added to the Al6061 after 15 and 30 h from the beginning of milling. The milling times with Al₂O₃ in these two samples were then 15 h and 30 min, respectively. Additionally, 3 vol.% Al₂O₃ (1 μm and 60 μm) was added to the Al6061 after 15 h of milling; where, the micron size Al₂O₃ in these two samples, was milled 15 h with the matrix. Hot pressing of milled samples was executed at 400 °C under 128 MPa pressure in a uniaxial die. The hot pressed samples were characterized by micro-hardness test, bulk density measurements, pin on disc wear test, and finally scanning electron microscopy observations. Fifteen hour-milled nanocomposite with nanoscale Al₂O₃, showed improvement in wear resistance and bulk density compared with that of 30 min-milled nanocomposites due to better dispersion of Al₂O₃ nanoparticles, improved surface quality of nanocomposite particles before pressing and more grain refinement of Al matrix. Moreover, increasing the reinforcement size increased the wear rate because of reduction in relative density, hardness and inter-particle spacing.     

Strength of β-sialon/Si3N4 layered composites

The strength of layered composites consisting of -sialon and Si3N4 layers, which were prepared by hot pressing, was investigated. The strength increased as the thickness of the sialon (outer layer) decreased, and reached almost the same level of Si3N4 (inner layer) when the sialon thickness was 250–300 m. No specific fracture morphologies were recognized around the interface of sialon and Si3N4. The aluminium concentration changed sharply around the interface, while the yttrium tended to diffuse deeper than aluminium. This tendency was remarkable in the samples hot-pressed at higher temperature (1900°C). The existence of compressive residual stress in the surface sialon layer was revealed and the residual stress increased as the sialon thickness decreased down to 250–300 m. The increase of strength with the decrease of sialon thickness was discussed based on the mechanical calculations in which the residual stress was considered. This calculation approximately agreed with the results of the samples hot-pressed at lower temperature (1800°C). However, the strength of the samples hot-pressed at 1900°C was much higher than the prediction in the thin range of the sialon thickness. The deep diffusion of yttrium into the sialon layers was thought to be one of the causes of this unpredictable effect.     

Optical properties of SPS-ed Y- and (Dy,Y)-α-sialon ceramics

Y_0.67Si₉Al₃ON₁₅ and Dy_0.4Y_0.3Si_8.85Al_3.15O_1.05N_14.95 ceramics were prepared by Spark Plasma Sintering (SPS) with and without heat treatment at 1700°C for 7 h or 17 h, and their optical transmittance were investigated over the wavenumber range 4000–1500 cm^–1. The results showed that the assemblages of the SPS-ed samples consisted of single crystallized -sialon phase in both compositions. EDS analysis indicated that -sialon was mainly stabilized by Dy³⁺ in the multi-cation (Dy,Y)--sialon composition. The SPS-ed specimens showed relatively high optical transmission properties, and the maximum transmittance reached around 65% at 2800 cm^–1 for 0.5 mm thick specimens of both compositions. The 7 h heat treatment caused the formation of small amount of melilite phase, resulting in non-uniform microstructure and decrease in optical transmittance. Extended heat treatment for 17 h led to more homogenous microstructure and increased the transmittance to some extent. Less melilite was formed in the multi-cation (Dy,Y)--sialon composition than in the single cation Y--sialon after heat treatment, and the transmittance of (Dy,Y)--sialon was also higher than that of Y--sialon.     

Carbothermal formation of β′-sialon from kaolinite and halloysite studied by 29Si and 27Al solid state MAS NMR

²⁷Al and ²⁹Si magic-angle spinning(MAS) nuclear magnetic resonance(NMR)and complementary X-ray diffraction (XRD) studies of carbothermal formation of sialons from kaolinite and halloysite confirm that the reaction involves the initial formation of mullite (3Al₂O₃·2SiO₂) and amorphous silica. In the presence of carbon, Si-N bonds are formed at 1200 °C, giving a continuum of silicon oxynitride compositions which become progressively more N-rich. These do not become sufficiently ordered to be detected by XRD until later in the reaction, when crystalline silicon oxynitride, possibly containing a little Al (O-sialon) and x-phase sialon are formed, followed by -sialon. The O- and x-phase sialons are transitory, but the -sialon persists throughout the reaction. Si-O bonds survive the destruction of the mullite and persist throughout the reaction, especially with kaolinite starting material. The ²⁹Si MAS NMR results indicate that Si-C bonds are formed later in the reaction than previously suggested, the SiC phase behaving more like a secondary product than a transitory intermediate. Al-N bonds are not detectable by ²⁷Al MAS NMR until very late in the reaction (after 8 h firing at 1400 °C), and coincide with the appearance of the secondary product AlN. The implications for the carbothermal reaction sequence in kaolinite and halloysite are discussed.     

Microstructural evolution of oxide-dispersion-strengthened Fe–Cr model steels during mechanical milling and subsequent hot pressing

Oxide-dispersion-strengthened (ODS) ferritic steels of Fe–9Cr–0.3Y₂O₃ and Fe–9Cr–0.2Ti–0.3Y₂O₃ (in mass) incorporating nanoscale oxide particles, were produced by mechanical milling (MM) followed by hot pressing (HP). Microstructural evolution of these two types of ODS steels were structurally characterized at each step of the elaboration processes by means of scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), and optical microscope. The observations of structure of the mixed powders and the nanoscale oxide particles in both ODS steels after MM indicate that the initial powders, coupled with the original yttria powders, get fractured by severe plastic deformation and ultrafine bcc grains (~20 nm) of the matrix and Y₂O₃ nanocrystals with irregular edges are formed during MM. The addition of titanium (Ti) promotes the refinement of bcc grains, Y₂O₃ nanocrystals and the formation of amorphous phase of Y₂O₃ during MM. TEM observations of these two Oxide-dispersion-strengthened (ODS) steels exhibit a very fine structure of micrometer-scale grains in which large number of nanoscale oxide particles are distributed after HP process. The observation of some unreinforced domains without the nanoscale oxide particles indicates that there still exist inhomogeneous areas, although the size of those oxide particles reaches nanoscale. Threshold stress of the HPped Fe–9Cr–0.2Ti–0.3Y₂O₃ steel with the relatively homogeneous dispersion was carefully evaluated on the basis of higher magnified images of the nanoscale oxide particles. Different values of threshold stress were obtained due to the various dispersions of the nanoscale oxide particles within different areas. That may be the reason why the threshold stress cannot be clearly obtained by the results of creep tests.     

Thermal stability and mechanical performance of multiply heat-treated α-sialon ceramics densified with rare earth oxides

Typical -sialon starting compositions, of formula Ln_0.33Si_9.3Al_2.7O_1.7N_14.3, were densified by hot-pressing using Ln₂O₃ as sintering additives, where Ln = Nd, Dy, and Yb. The as-sintered materials were heat-treated at 1450°C for 96 hours and then re-sintered at 1800°C for 1 hour to observe the overlapping effects of both Ln₂O₃ and multiple heat-treatment on thermal stability of the Ln--sialon phase and also the change in microstructure. The kinds of grain boundary phases which occurred also affected the results. The hardness, fracture toughness and flexural strength of the materials were evaluated using indentation and three-point bending tests, respectively. Mechanical tests and detailed microstructural analysis have led to the conclusion that a multiple-mechanism is involved, with debonding, crack deflection, crack bridging, and elongated grain pull-out all making a significant contribution towards improving the fracture toughness. Nd-containing specimens were tough with a highest indentation fracture toughness K_1C of 7.0 MPa m^1/2. In contrast, Dy- and Yb-containing specimens were hard and brittle with a highest Vickers hardness H_V10 of 18.0 GPa. All re-sintered specimens underwent transformation to some degree, leading to a degradation of mechanical properties as a consequence.     

Carbothermal production of β′-sialon from alumina,silica and carbon mixture

Mixtures of pure nanometer-sized amorphous silica and -alumina with the atomic ratio SiAl=1 were reduced by a stoichiometric amount of carbon between 1100 and 1450 °C in flowing nitrogen in order to produce -sialon powder. Using aqueous suspensions of starting materials, compacts with different microstructures were prepared for reaction. Silica reduction to SiO occurred at a temperature as low as 1300 °C and part of it was removed with flowing nitrogen. Carbothermal reaction involving nitrogen stated at 1350 °C and Si₂N₂O was found as an intermediate together with SiC, resulting in -sialon formation. Loss of silica from the system led to AlN formation. Decomposition of -sialon into sialon polytypoids (15R, 12H) was observed as a result of sialon and AlN reaction at 1450 °C. The reaction rate of sialon formation was slowed down compared to the carbothermal reduction of kaolin because of the lack of impurities. The microstructure of the reacted pellets influenced the reaction products, and the narrow pore size distribution as well as good homogeneity enhanced -sialon formation.On leave, from Silesian Technical University, Krasiskiego 8, 40-019 Katowice, Poland.     

Phase relationship between β′- and O′-sialon at 1623 K

-sialon whiskers and co-products of synthesis, such as -sialon powders and O-sialon powders, were annealed at 1623 K for 8 h in a closed graphite reaction tube under 1 atm nitrogen. Phase stabilities, Si/Al ratios, and crystallographic features were investigated. The O-sialon phase, which formed in the early stage of synthesis when oxygen partial pressure was relatively high, became less stable in the present annealing condition and decomposed. The majority of released aluminium and possibly oxygen from the decomposed O-powder was incorporated into -sialon whiskers with little change in its lattice parameters, when the -sialon whiskers were included in annealing. The aluminium contents were always lower in the -whiskers than in the powders even after increasing its aluminium content during 8 h annealing. The lattice parameters of both -whiskers and powders increased with increasing aluminium content and became closer after annealing. The lattice parameters of -whiskers remained the same before and after annealing despite the increased aluminium content, while the lattice parameters of -powders decreased despite its aluminium content remaining unchanged. The lattice parameters of O-sialon increased with increasing aluminium content, and the increase in thea direction is the largest when compared with other parameters.     

The reaction hot-pressing of compositions in the system Al-Si-N-O corresponding to β′-sialon

The reaction hot-pressing at 1700 and 1750° C of a number of compositions in the system Al-Si-N-O corresponding to points spanning the-sialon phase line in the region of z=0.8 has been studied. Measurements have been made of densification rate and of the rate of conversion of-Si₃N₄ to-sialon. The densification process for these compositions may be described in terms of a liquid-phase assisted fast particle rearrangement process succeeded by Coble creep. The rates of these processes are sensitive to the volume of grain-boundary liquid phase present, which in turn is determined by the position of the compositional point in relation to the-sialon line. For systems containing very little grain-boundary phase, the vapour-phase transport of material may become important.