The role of dispersed particles in strengthening and fracture mechanisms in a Mo-ZrC alloy processed by mechanical alloying

The tensile properties of a ZrC particle-dispersed Mo, which was processed by spark plasma sintering with mechanically alloyed powder, were investigated at room temperature and at elevated temperatures of 1170 to 1970 K. The Mo-ZrC alloy showed much higher strength at room temperature than a fully recrystallized pure Mo. The high strength of Mo-ZrC is mainly attributed to a very small grain size (about 3 μm). The main role of the ZrC particle is not to increase strength due to the particle-dislocation interaction, but to limit grain growth during sintering and to attain the very small grain size. The elongation at room temperature of Mo-ZrC was much lower than that of pure Mo. This is probably related to the higher interstitial contents. However, Mo-ZrC showed a large elongation of 180 pct at 1970 K and 6.7×10⁻⁴ s⁻¹. It was suggested that the ZrC particles stabilized the fine-grained microstructure yet provided no cavitation sites at 1970 K; as a result, the large elongation was attained.     

Modification of the sintering kinetics of palladium by a surface oxide

The presence of a surface oxide layer on palladium powders gives rise to a densification-free sintering process controlled by a surface diffusion mechanism with an activation energy of 59.2 kJ/mol₋₁. At temperatures above the oxide dissociation temperature in air, 1062 K, palladium powders sinter with an activation energy of 120.4 kJ/mol"1, indicative of a grain boundary diffusion. AtT < 1061 K and under a 10₋₈ atm vacuum, sintered powders showed densification but with an activation energy too high to be grain boundary diffusion-related. These results are interpreted in terms of the role of the surface oxide and are compared with previously published results on the sintering of Pd.     

Processing and Characterization of Cu-Al-Ni Shape Memory Alloy Strips Prepared from Prealloyed Powder by Hot Densification Rolling of Powder Preforms

The present work deals with the preparation of near-full density Cu-Al-Ni shape memory alloy (SMA) strips from argon-atomized prealloyed powder via a powder metallurgy (PM) route comprising cold die compaction to prepare powder preforms, sintering, and hot densification rolling of unsheathed sintered powder preforms under protective atmosphere at 1273 K (1000 °C). It has been shown that argon-atomized spherical Cu-Al-Ni SMA powder consisted of very fine equiaxed grains and no appreciable grain growth occurred during sintering at 1273 K (1000 °C). It also has been shown that no appreciable densification occurred during sintering, and densification was primarily achieved by hot rolling. The densification behavior of the sintered powder preforms during hot rolling was discussed. The hot-rolled Cu-Al-Ni strips were heat-treated at 1223 K (950 °C) for 60 minutes and water quenched. The heat-treated strips consisted of equiaxed grains with average size approximately 90 μm. The heat-treated Cu-Al-Ni SMA strips consisted of self-accommodated b₁^￠ \beta_{1}^{'} martensite primarily, and showed smooth b₁ T b₁^￠ \beta_{1} \Rightarrow \beta_{1}^{'} transformation behavior coupled with a very low hysteresis (≈25 K (25 °C)). The heat-treated strips exhibited an extremely good combination of mechanical properties with fracture strength of 530 MPa and 12.3 pct fracture strain. The mode of fracture in the finished strip was primarily void-coalescence-type ductile together with some brittle transgranular type. The shape memory tests showed almost 100 pct one-way shape recovery after 100 bending-unconstrained heating cycles at 4 pct applied prestrain, exhibiting good stability of Cu-Al-Ni strips under thermomechanical actuation cycling. The two-way shape memory strain was found approximately 0.45 pct after 15 training cycles at 4 pct training strain.     

Studies on hot deformation of sintered cobalt

The hot deformation behavior of sintered cobalt powder was studied. The Co powder prepared by thermal decomposition of cobalt oxalate was subsequently compacted by cold isostatic pressing (CIP) and sintered at 1300 °C under H₂ atmosphere. Cobalt rods of 95 pct theoretical density were obtained. Strain rate change tests in compression were conducted in the temperature range of 900 °C to 1300 °C by changing strain rates from 0.001 to 3.2 s⁻¹. Uninterrupted hot compression tests at constant strain rates and selective temperatures were also conducted. Microcracks as well as surface cracks were observed in the samples tested below 1200 °C. It was observed that the strain rate sensitivity (SRS) increased with increasing temperature and decreasing strain rate, with the maximum SRS of 0.3 being obtained at 1285 °C and strain rate of 10⁻³ s⁻¹. Despite the higher SRS at low strain rates, the hot workability of sintered cobalt was found to be poor. Extensive grain boundary microcracking was observed, with the density being lowered after deformation. However, the samples tested at higher strain rates showed less microcracking and an increase in density. On the basis of the results, it was concluded that ease of grain boundary sliding at lower strain rates and higher temperatures was responsible for the poor workability at these conditions.     

掺杂氧化铝对纳米钨粉烧结过程的影响

以碳热预还原和氢气深还原两步制备的纳米钨粉作为烧结原料,即先通过碳黑还原脱除三氧化钨中的大部分氧,再以氢还原脱除残留的氧。该方法制备的钨粉颗粒呈球形形貌,平均晶粒度可达90 nm。同时,向钨粉中掺杂质量分数为1%和2%的氧化铝,探究了氧化铝对钨粉烧结行为的影响。通过烧结样品的断口形貌和晶粒的平均尺寸分析发现,氧化铝对烧结后期的晶粒长大有明显的抑制作用,相同的烧结温度下晶粒的尺寸随着氧化铝含量的上升而减小。在1600 ℃时,纯钨粉烧结坯的晶粒平均尺寸为2.75 μm,但添加质量分数为1%和2%氧化铝的烧结样品晶粒平均尺寸约为1.5 μm,这是由于氧化铝能有效地抑制烧结后期的钨粉晶粒长大。纯钨粉和掺杂氧化铝钨粉的烧结坯的硬度随温度升高具有不同的趋势。掺杂钨粉烧结坯的硬度随着温度的升高而升高,且其最大值高于800 HV。但是,纯钨粉烧结坯的硬度随烧结温度增加而先增加后降低,在1400 ℃时取得最大值（473.6 HV）,这是由纯钨粉烧结坯的晶粒在高温下急剧长大所导致。在烧结温度为1600 ℃时,纯钨粉、掺杂质量分数1%和2%的氧化铝掺杂的钨粉的烧结坯的相对密度依次为98.52%、95.43%和93.5%。      

Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5/FeAl2 powders Part 1: Experimentation and results

Abstract

High density Fe₃Al was produced through transient liquid phase sintering, using rapid heating rates of greater than 150 K min^-1 and a mixture of prealloyed and elemental powders. Prealloyed Fe₂Al₅/FeAl₂ (50Fe/50Al, wt-%) powder was added to elemental iron powder in a ratio appropriate for producing an overall Fe₃Al (13·87 wt-%) ratio. The heating rate, sintering time, sintering temperature, green density and powder particle size were controlled during the study. Heating rate, sintering time and powder particle size had the most significant influence upon the sintered density of the compacts. The highest sintered density of 6·12 Mg m^-3 (92% of the theoretical density for Fe3Al) was achieved after 15 minutes of sintering at 1350°C, using a 250 K min^{- 1} heating rate, 1-6 μm Fe powders and 5·66 μm alloy powders.

SEM microscopy suggests that agglomerated Fe₂Al₅/ FeAl₂ particles, which form a liquid during sintering, are responsible for a significant portion of the remaining porosity in high sintered density compacts, creating stable pores, larger than 100 μm diameter, after melting. High density was achieved by minimising the Kirkendall porosity formed during heating by unbalanced diffusion and solubility between the iron and Fe₂Al₅/FeAl₂ components. The lower diffusion rate of aluminium in the prealloyed powder into the iron compared with elemental aluminium in iron, coupled with a fast heating rate, is expected to permit minimal iron-aluminium interdiffusion during heating so that when a liquid forms the aluminium dissolves in the iron to promote solidification at a lower aluminium content. This leads to a further reduction in porosity.     

Elevated temperature deformation behavior of an Al-8.4 wt pct Fe-3.6 wt pct Ce alloy

The elevated temperature deformation characteristics of a rapidly solidified Al-8.4 wt pct Fe-3.6 wt pct Ce alloy have been investigated. Constant true strain rate compression tests were performed between 523 and 823 K at strain rates ranging from 10⁻⁶ to 10⁻³ s⁻¹. At temperatures below approximately 723 K, the alloy is significantly stronger than oxide dispersion strengthened (ODS) aluminum. However, at higher temperatures, the strength of the Al-Fe-Ce alloy falls rapidly with increasing temperature while ODS aluminum exhibits an apparent threshold stress. It is shown that particle coarsening cannot fully account for the reduction in strength of the Al-Fe-Ce alloy at elevated temperatures. The true activation energy for deformation of the Al-Fe-Ce alloy at temperatures between 723 and 773 K is significantly greater than that for self-diffusion in the matrix. This is unlike the behavior of ODS alloys, which contain nondeformable particles and exhibit true activation energies close to that for self-diffusion in the matrix. Since abnormally high true activation energies for deformation are also exhibited by materials containing deformable particles, such as γ^′ strengthened superalloys, it is concluded that elevated temperature deformation in ythe Al-Fe-Ce alloy involves deformation of both the matrix and the precipitates. The loss of strength of the Al-Fe-Ce alloy appears to be related to a reduction in strength of at least some of the second phase particles at temperatures above 723 K. Formerly Research Assistant, Department of Materials Science and Engineering, Stanford University.     

Improved densification of carbonyl iron compacts by the addition of fine alumina powders

An investigation of the effect of alumina particles on the sintering behavior of a carbonyl iron powder compact was carried out in this study. Two different-sized alumina, 0.05 and 0.4 μm, were added to the iron compact at amounts up to 1.2 wt pct. When 0.4 μm alumina particles were added, no sintering enhancement was observed. But, in contrast to previous results reported in literature, the addition of 0.1 to 0.2 wt pct of 0.05 μm alumina particles was found to improve the densification. With 0.1 wt pct, the sintered density increased from 7.25 to 7.40 g/cm³ after the compact was sintered at 1350 °C for 1 hour in hydrogen. Dilatometric curves showed that alumina impeded the early-stage sintering of iron in the α phase, but improved densification in the γ phase at high temperatures. These results, along with microstructural analysis, suggested that alumina particles exhibit dual roles; their physical presence blocks the diffusion of iron atoms, thus causing inhibition of sintering, while their grainboundary pinning effect prevents exaggerated grain growth of iron and helps densification. It follows that, depending upon the amount and size of the alumina powders, either an increase or decrease in the final sintered density can be obtained.     

Design and fabrication of W-Mo-Ti-TiAl-Al system functionally graded material

To obtain a kind of functionally graded material (FGM) with a density gradient, the W-Mo-Ti-TiAl-Al system graded material was designed, and the powder metallurgy method was chosen for its fabrication. The sintering of W, W-Mo, and Mo-Ti alloys at low temperature was studied, and then the approximately wholly dense W-Mo-Ti-TiAl system FGM was achieved by one-step sintering at 1473 K for 1 hour under a pressure of 30 MPa. It was found that through sintering at 1473 K, mainly the mechanical mixtures of W and Mo were formed in W-Mo alloys. In Mo-Ti alloys, the newly designed Fe-Al sintering aids not only have an important effect on the densification of the alloys, but also contribute to the formation of the (Mo, Ti) solid solution. However, the solid-solution reaction that occurred in Mo-Ti alloys was still insufficient. During the sintering of Ti + TiAl, the chemical reaction of Ti + TiAl → AlTi₂ was induced within the sintered body. The W-Mo-Ti-TiAl-Al system FGM was finally fabricated by joining of the TiAl side of the sintered W-Mo-Ti-TiAl system FGM to metal Al with an Al-based brazing filler metal, and its density changed quasi-continuously within the large range from 17.15 to 2.70 g/cm³.     

THE PREPARATION AND SOME PROPERTIES OF CHROMIC OXIDE-CHROMIUM CERMETS.

Abstract

Compacts of chromium oxide/chromium mixtures have been sintered in vacuum at temperatures up to 1600°C to produce cermets. Two types of chromium powder were used—an electrolytic and an aluminothermic powder. The effect of chromium content and of sintering temperature on the sintered density and microstructure has been studied and supplemented by tests of hardness and compressive strength.

Considerable densification was achieved by additions of chromium in the range 1–50 wt.-%, with the optimum content at 5–10%. Compressive strengths < 10 tons/in² were attained over a wide range of composition.     

The oxidation-reduction kinetics of palladium powder

The cyclic oxidation-reduction of submicrometer sized palladium powder was investigated over the temperature range 848 to 923 K. The total oxygen uptake was found to decrease with increasing number of cycles as a consequence of sintering. Furthermore, sintering was found to be restricted to the reduction steps in these cycles. The relationships for the rate constants of the oxidation and reduction processes are, respectively, K_x, = (1.04)10⁶ exp[-(74.1)10³/RT],k _r = (7.63)10¹² exp[—(207.9)10³/RT]. The activation energies for the oxidation of palladium powder and the reduction of palladium oxide are 74.1 and 207.9 kJ mol⁻¹, respectively.     

微波烧结制备ITO靶材的工艺

采用单相ITO(indium tin oxide,铟锡氧化物)复合粉末,经过压制成形后,在纯氧气氛下微波烧结制备ITO靶材,研究烧结温度、保温时间和压制压力等主要工艺参数对ITO靶材致密化的影响。结果表明:靶材的相对密度随烧结温度升高而增大;在1 600℃烧结时,靶材的相对密度随保温时间增加先增大后减小,在保温1.5 h时相对密度达到最大值(98.67%),高温长时间烧结对ITO靶材的致密化不利。微波烧结的ITO靶材显微组织均匀,晶粒尺寸较均匀,约为6～8μm。不同温度下制备的ITO靶材均无SnO2相析出,仍是单一的固溶体相,不存在第二相。     

The chemical diffusivity of oxygen in liquid iron oxide and a calcium ferrite

Measurements have been made of the chemical diffusion coefficient of oxygen in liquid iron oxide at temperatures from 1673 to 1888 K and in a calcium ferrite (Fe/Ca = 2.57) at temperatures from 1573 to 1873 K. A gravimetric method was used to measure the oxygen uptake during the oxidation of the melts by oxygen or CO₂-CO mixtures. The rate was shown to be controlled by mass transfer in the liquid melt. The chemical diffusivity of oxygen in liquid iron oxide at oxygen potential between air and oxygen was found to be 4.2±0.3 × 10⁻³ cm²/s at 1888 K. That in iron oxide at oxidation state close to iron saturation was established to be given by the empirical expression log D=−6220/T + 1.12 for temperatures between 1673 and 1773 K. For the calcium ferrite (Fe/Ca=2.57) at oxygen potential between air and oxygen, the diffusivity of oxygen was found to be given by log D=−1760/T−1.31 for temperatures between 1673 and 1873 K. This article is based on a presentation made in the “Geoffrey Belton Memorial Symposium,” held in January 2000, in Sydney, Australia, under the joint sponsorship of ISS and TMS.     

Effect of surface oxide films on the properties of pulse electric-current sintered metal powders

Metallic powders with various thermodynamic stability oxide films (Ag, Cu, and Al powders) were sintered using a pulse electric-current sintering (PECS) process. Behavior of oxide films at powder surfaces and their effect on the sintering properties were investigated. The results showed that the sintering properties of metallic powders in the PECS process were subject to the thermodynamic stability of oxide films at particles surfaces. The oxide films at Ag powder surfaces are decomposed during sintering with the contact region between the particles being metal/metal bond. The oxide films at Cu powder surfaces are mainly broken via loading pressure at a low sintering temperature. At a high sintering temperature, they are mainly dissolved in the parent metal, and the contact regions turn into the direct metal/metal bonding. Excellent sintering properties can be received. The oxide films at Al powder surfaces are very stable, and cannot be decomposed and dissolved, but broken by plastic deformation of particles under loading pressure at experimental temperatures. The interface between particles is partially bonded via the direct metal/metal bonding making it difficult to achieve good sintered properties.     

IRON-COPPER-TIN SINTERED COMPACTS

Abstract

A wide range of copper and tin powder additions to iron powder sintered compacts hasbeen studied. From mechanical-property tests it has been shown that when using sinteririg temperatures of 900–1100°C in nitrogen/10% hydrogen atmospheres there is an optimum copper: tin ratio of 15:2. The mechanical properties obtained from compacts pressed from iron mixed with 4% copper+tin in this ratio and sintered at 900°C were similar to those obtained from iron ?l0% copper powder compacts sintered at 1100°C. Moreover, the iron-copper-tin components showed improved dimensional accuracy.

In a further series of experiments, it was shown that tin additions to iron-copper alloy compacts increased the solubility of iron in the liquid phase at the sintering temperature and simultaneously decreased the rate of diffusion of copper into the iron particles. At the same time, tin improved the wettability of the liquid, reducing its surface tension and allowing it to disperse more completely throughout the matrix. The mechanical properties of compacts containing larger amounts of tin were decreased by the presence of brittle compounds, although the sintering rate was increased. It is concluded that the optimum properties of iron-copper-tin compacts are obtained by making correct additions of copper and tin to the iron powder and giving careful consideration to the sintering atmosphere.     

Rapid sintering of iron powders under action of electric field

Abstract

A new rapid sintering technique for iron powders compacted under the action of an electric field with high current density has been advanced. The results show that the sintering densification of iron powder could be finished in less than 6 min at a temperature of 800^u C reached at a heating rate of 600 K s^?1, and the relative density of the sintered compact was over 95%. Moreover, the sintering densification was almost finished in the heating stage of the compact.     

STUDIES ON THE ACTIVATION-SINTERING OF IRON POWDER

Abstract

A study of the sintering behaviour of iron compacts containing additions of tin up to 1 wt.-% has been made. A tensile strength of 234 MN/m² (34 x 10³ lbf/in²) has been achieved with an optimum tin addition of 0·5 wt.-%, sintering being carried out for 10 min at 1100°C (1373 K) in a reactive halide atmosphere. Combination of the two ‘activating’ techniques (addition of tin and sintering in a reactive atmosphere) permits current properties to be attained at considerably lower sintering temperatures or sintered densities, and is much more effective than when they are applied individually. A tensile strength of 165·3 MN/m² (24 x 10³lbf/in²), achieved by sintering at 1200°C (1473 K) for 10 min with an addition of 0·5 wt.-% tin can be obtained by reactive-sintering the same composition at 900°C (1173 K) for 10 min. Alternatively, the density of the part can be reduced from 6·7 to 6·2 g/cm³ with no loss of strength or elongation. Tin in excess of 0·5 wt.-% causes deterioration in properties under the sintering conditions studied and a reason for this is cited. The improvements in properties are lost also if admixed lubricant is used in the compactionprocess.     

A study on the improvement of the sintered density of W-Ni-Mn heavy alloy

Liquid phase sintering behavior of 90W-6Ni-4Mn heavy alloy has been studied. The present work takes into account the thermodynamic oxidation/reduction reactions of the constituent elements W, Ni, and Mn. The sintering cycle consists of heating under high purity nitrogen gas, holding at reduction temperatures after the atmosphere is changed to dry hydrogen, and sintering at 1260 °C for 1 hour. As the reduction temperature increases from 1050 °C to 1200 °C, the relative sintered density increases from 92 pct, reaching 100 pct at temperatures above 1150 °C. The relative density increases with increasing holding time at the reduction temperature and remains unchanged with heating rate. The sintered microstructure has been analyzed by a scanning electron microscope and energy dispersive X-ray spectroscopy. The relative density was compared with those obtained from other investigators. It is found that the formation of manganese oxide due to reducing reactions of W and Ni powders should be avoided in order to obtain a W-Ni-Mn heavy alloy without pores.     

Spark plasma sintering of Al-Si-Cu-Fe quasi-crystalline powder

This article presents the results of a study on the microstructure and mechanical properties of Al−Si−Cu−Fe specimens produced by the spark plasma sintering (SPS) technique. The microstructure of the starting powder and bulk specimens was analyzed by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The formation of the icosahedral and decagonal quasi-crystalline phases in the as-gas-atomized powders is described for the first time. It is then shown that these metastable phases transformed into the 1/1 cubicapproximant phase upon heating at about 600°C. Second, the effects of SPS process parameters such as the temperature and time have been investigated. Owing to the generation of a spark discharge neighboring powder particles, dense cylindrical samples were obtained after a short sintering time of 30 minutes at the temperature of 650°C. The highest values of the Vickers microhardness, about 8.9 GPa, were obtained when the powders were sintered in the temperature range of 600°C to 650°C for a holding time of 30 minutes, while the fracture toughness was found to be inversely proportional to the sintering temperature. However, at the sintering temperature of 650°C, the fracture toughness increased from about 1.40 to 1.52 MPa √m as the holding time increased from 10 to 60 minutes. As compared to cast specimens, the enhanced mechanical properties are explained by the refined microstructure resulting from the low temperature and short sintering time applied during SPS processing     

A sintering study on the β-spodumene-based glass ceramics prepared from gel-derived precursor powders with LiF additive

Beta-spodumene (Li₂O·Al₂O₃·4SiO₂, LAS) powders were prepared by a sol-gel process using Si(OC₂H₅)₄, Al(OC₄H₉)₃, and LiNO₃ as precursors and LiF as a sintering aid agent. Dilatometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and electron diffraction (ED) were utilized to study the sintering, phase transformation, microstructure, and properties of the β-spodumene glass-ceramics prepared from the gel-derived precursor powders with and without LiF additives. For the LAS precursor powders containing no LiF, the only crystalline phase obtained was β-spodumene. For the pellets containing less than 4 wt pct LiF and sintered at 1050 °C for 5 hours the crystalline phases were β-spodumene and β-eucryptite (Li₂O·Al₂O₃·2SiO₂). When the LiF content was 5 wt pct and the sintering process was carried out at 1050 °C for 5 hours, the crystalline phases were β-spodumene, β-eucryptite (triclinic), and eucryptite (rhombohedral (hex.)) phases. With the LiF additive increased from 0.5 to 4 wt pct and sintering at 1050 °C for 5 hours, the open porosity of the sintered bodies decrease from 30 to 2.1 pct. The grains size is about to 4 to 5 μm when pellect LAS compact contains LiF 3 wt pct as sintered at 1050 °C for 5 hours. The grains size grew to 8 to 25 μm with a remarkable discontinuous grain growth for pellet LAS compact contain LiF 5 wt pct sintered at 1050 °C for 5 hours. Relative densities greater than 90 pct could be obtained for the LAS precursor powders with LiF > 2 wt pct when sintered at 1050 °C for 5 hours. The coefficient of thermal expansion of the sintered bodies decreased from 8.3 × 10⁻⁷ to 5.2 × 10⁻⁷/°C (25 °C to 900 °C) as the LiF addition increased from 0 to 5 wt pct.