Cold compaction of polyether-etherketone and nickel powder blends

This study deals with the cold compaction of polyether-etherketone (PEEK) and nickel powder blends. Four different types of PEEK powders which are commercially available from Imperial Chemical Industries (ICI) were utilized for this investigation. These PEEK powders included fine and coarse size powders of a low viscosity grade (150PF and 150P) and similar powders of a high viscosity grade (450PF and 450P). Each of the four different PEEK powders were blended with about 10 vol?% nickel powder (Novamet) using a dry mixing technique. These PEEK/nickel powder blends were then successfully compacted at room temperature. Green strengths as high as 39.5 MPa and 26.3 MPa were measured on nickel filled 150 grade and 450 grade compacts, respectively. The higher strength values of the nickel filled compacts compared to their respective unfilled ones were attributed to a higher degree of mechanical interlocking and plastic deformation, which was induced in the polymer particles during compaction by the hard nickel filler. These composites also exhibited lower viscoelastic recoveries than their respective unfilled compacts. Electrical resistivities as low as 0.06 ohm-cm were achieved by compacting 150P/nickel powder blends. This resistivity value agreed well with the calculated value predicted from the literature.     

Sintering high performance semicrystalline polymeric powders

Poly(ether ether ketone) (PEEK) is high performance semicrystalline thermoplastic with a glass transition temperature of 143°C. The melting point (Tm) is quoted as 334°C. Because of its high thermal transitions, PEEK, requires high temperatures for processing, at least 370–400°C. It has been determined that under the recommended processing conditions PEEK can undergo branching and eventually crosslinks. An alternative to melt processing PEEK is to apply the powder metallurgy technique of sintering. This involves cold (room temperature) compaction of the polymeric powder, followed by pressure free sintering of the resultant green body. We have reported a process for preparing submicron PEEK particles, and the focus here is on the free sintering of these particles with emphsis on the effects of particle size, sintering temperature, and compaction pressure. The data is evaluated using the two particle model developed by Frenkel as well as the crack healing theory developed by Wool.     

Dependence of Compaction Efficiency in Dry Pressing on the Particle Size Distribution

The compact densification with pressing pressure (compaction efficiency) was determined to be sensitive to the particle size distribution. For the three types of alumina powders used in this research, the compaction efficiency increased with increasing particle size. It has been demonstrated that if the compact density versus log (pressure) has a linear relationship for any two types of powders, so do the blends of the two powders. A model is proposed which can predict the compaction efficiency of a binary particle system based on the Furnas particle packing model and consider the packing efficiency as a function of forming pressure. The composition of the binary mixture at which the highest density is obtained under high pressures is also the composition having the largest compaction efficiency. When coarse particles were added to this composition, the compaction efficiency slowly decreased, and when fine particles were added, the compaction efficiency rapidly decreased. For a continuous particle size distribution, the highest compaction efficiency is related to the average value of -log (porefraction).     

Mechanical and Thermal Properties of Poly(phthalazinone biphenyl ether sulfone)/PEEK Blends

A series of blends with various compositions are prepared by melt extrusion on the basis of novel copoly(phthalazinone biphenyl ether sulfone) (PPBES) and poly(ether ether ketone) (PEEK). The melt flowability, mechanical and thermal properties of the blends are studied. The results show that the incorporated PEEK has a large influence on the melt viscosity and thermal stability of blends. The tensile strength of the blends remains at about 90 MPa at room temperature; PPBES improves the mechanical properties of PEEK at 150°C. The flexural strength and modulus of the PPBES/PEEK blends also increase with the addition of PEEK.     

Fine poly(ether ether ketone) powders

The physical form of polymers is often important for carrying out subsequent processing operations. For example, fine powders are desirable for molding and sintering compounds because they consolidate to produce void free components. The objective of this work is to prepare fine polymeric particulates suitable for processing into fiber reinforced polymer matrix composites. Micron size particles of poly(ether ether ketone) (PEEK) were prepared by rapidly quenching solutions of these materials. PEEK pellets were dissolved at temperatures near the PEEK melting point in a mixture of terphenyls and quaterphenyls; then the solution was quenched to a temperature between the T_g and T_m (≈ 225°C) by adding a room temperature eutectic mixture of diphenyl ether and biphenyl. A supersaturated, metastable solution of PEEK resulted, causing rapid nucleation. Fine PEEK particles rapidly crystallized from this solution. The average particle size was measured using transmission electron microscopy, atomic force microscopy, and by light scattering of aqueous suspensions which had been fractionated by centrifugation. The average particle diameter was about 0.6 μm. Three dimensional photomicrographs obtained via atomic force microscopy showed some aggregates in the suspensions. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 63: 1571–1578, 1997     

Densification of nanocrystalline MgO ceramics by hot-pressing

Densification of pure nanocrystalline MgO powder with 10 nm particle size by hot-pressing was investigated in the temperature range 700–800 °C, applied pressure range 100–200 MPa, and for durations of up to 240 min. It was shown that significant densification under the pressure begins above 440 °C. Densities higher than 99.5% with grain size of 73 nm were achieved at 790 °C and 150 MPa for a 30 min duration. Remarkable densification from 90 to 99.5% was observed by temperature change from 700 to 790 °C, for which the grain size was doubled only. The final grain size decreased with increasing the applied pressure. Higher shrinkage rates and cumulative shrinkages were recorded by the application of pressure at 550 °C rather than from room temperature. The temperature at which the pressure was applied is crucial in determining the maximum shrinkage rate in the nanocrystalline compacts. This effect was related to the morphological changes of the particles caused by plastic deformation at lower temperatures. Analysis of the densification rate and its comparison to the literature data was in agreement with Coble creep, where self-diffusion of Mg²⁺ cations along the grain boundaries acts as a main densification mechanism.     

Dielectric properties of barium titanate ceramics with different materials powder size

The dielectric properties of barium titanium ceramics fabricated with nano-size fine powders (about 40 nm) are compared with that fabricated with micro-size coarse powders (about 2 μm). Three kinds of ceramics were fabricated; one using pure nano-size fine powders, the other using pure micro-size coarse powders, and the third using the combination of both. The sintering temperature of the ceramics with pure nano-size fine powders is 150 °C lower than that with pure micro-size coarse powders. For the same sintering conditions, the relative density of the ceramics is increases with the amount of nano-size fine powders. The grain size of the ceramics body with pure micro-size coarse powder is about 5 μm, but that of pure nano-size fine powder is about 1 μm. The room temperature dielectric constant of the ceramics increases with the increasing of the amount of nano-size fine powder. For pure nano-size fine powders, the room temperature dielectric constant is about 5000, and that of micro-size coarse powders is about 2200.     

Compaction as a Critical Factor for Success in the Sintering of Ultra-Fine WC–Co Powders

Heat treatment of ultra-fine WC–13Co powders was carried out prior to cold compaction, in an attempt to improve the sintered density. The findings indicate that a preheat treatment of ultra-fine or nano-sized powders significantly improves the densification process. This study showed that a low compacting pressure, <200 MPa, can be effectively used through this technique to retain ultra-fine structure. The densification behavior of preheated powder was compared with the samples prepared by a conventional technique and explained with size distribution, standard deviation, and surface effect.     

ZrB2-MoSi2 ceramics: A comprehensive overview of microstructure and properties relationships. Part II: Mechanical properties

The mechanical behavior of ZrB₂-MoSi₂ ceramics made of ZrB₂ powder with three different particle sizes and MoSi₂ additions from 5 to 70 vol% was characterized up to 1500 °C. Microhardness (12–17 GPa), Young’s modulus (450–540 GPa) and shear modulus (190–240 GPa) decreased with both increasing MoSi₂ content and with decreasing ZrB₂ grain size. Room temperature fracture toughness was unaffected by grain size or silicide content, whilst at 1500 °C in air it increased with MoSi₂ and ZrB₂ grain size, from 4.1 to 8.7 MPa m^½. Room temperature strength did not trend with MoSi₂ content, but increased with decreasing ZrB₂ grain size from 440 to 590 MPa for the largest starting particle size to 700–800 MPa for the finest due to the decreasing size of surface grain pullout. At 1500 °C, flexure strength for ZrB₂ with MoSi₂ contents above 25 vol% were roughly constant, 400–450 MPa, whilst for lower content strength was controlled by oxidation damages. Strength for compositions made using fine and medium ZrB₂ powders increased with increasing MoSi₂ content, 250–450 MPa. Ceramics made with coarse ZrB₂ displayed the highest strengths, which decreased with increasing MoSi₂ content from 600 to 450 MPa.     

Densification of silicon nitride powder with various additives

Cold compaction behavior of a sub-micron size silicon nitride powder with additives has been studied at various loading rates up to about 450 MPa. Liquid lubricants are found to be more effective than the solid lubricants. A marked increase in relative density has been obtained with the aid of 10 weight percent polyethyleneglycol after surface treatment of the powder with a dispersant solution. The loading rate between 0.8 and 800 MPa per minute has no effect on the densification process. Results are analysed with various theoretical equations available in the literature. The Cooper and Eaton's equation and also its modified form are used to determine the mechanism of densification during cold compaction.     

Cold compaction molding and sintering of polystyrene

It is the objective of this paper to demonstrate the applicability of cold compaction molding followed by a sintering treatment to the processing of polystyrene powders. The influence of pressure, compaction speed, and peak pressure dwell time on the green (as compacted) density and the green tensile strength, as well as the effect of sintering on the tensile strength and dimensional change, were evaluated. The resulting data indicate that room temperature compaction alone is insufficient to provide adequate tensile strength for the compacts. Sintering the green compacts at temperatures of 150 to 173°C markedly improves the tensile strength while simultaneously causing a thickness change in the compacts. This thickness change results from gas evolution, pore shrinkage, and viscoelastic recovery of the residual stresses induced by pressure. For compacts of 0.225 in. thickness, an optimum sintering treatment of 173°C for 30 mins is recommended to provide a tensile strength of 4,000 psi and a thickness change of less than + 7 percent. Coining (repressing) the green compacts does not appreciably affect the sintered strength. However, a finer particle size improves the sintered properties. A review of the literature on the flow behavior of polystyrene suggests that a non-Newtonian viscous flow mechanism is followed by a Newtonian one as sintering progresses.     

Compaction and Sintering Behavior of Bimodal Alumina Powder Suspensions by Pressure Filtration

The compaction behavior of fine alumina powders with different particle sizes or bimodal particle-size distributions that are undergoing pressure filtration was investigated. Three alumina powders—average particle sizes of 0.2—0.86 μm—were compacted to a solids fraction of 62—65 vol% from suspensions at pH 3, which was the pH level at which the suspensions showed their lowest viscosity. When the powders of different average sizes were mixed, the suspensions showed better flowability, and the lowest viscosity was obtained when the fraction of fines was ∼30 vol% and pH = 3. The mixed-sized powder suspensions were compacted to higher density than the suspensions of unmixed fine or coarse powders, and the maximum density was obtained for mixed suspensions that had the lowest viscosity, despite the different particle-size ratio. Maximum densities of 72.5% and 75.0% were attained when the size ratios were 2 and 5, respectively. The compacts that were pressure-filtered from mixed suspensions exhibited a single-peaked pore-size distribution and a homogeneous microstructure, whereas the pore-size distributions of dry-pressed compacts were double-peaked. The sintering behavior of the compacts that were pressure-filtrated from bimodal powders exhibited significantly better sinterability and much-less linear shrinkage than the coarser powders and the dry-pressed powder compacts.     

Effect of Polyethylene Glycol (PEG) Powder on Compressibility and Microstructural Properties of Sintered α-Alumina

This study examines the effect of various contents of polyethylene glycol (PEG) powders on density, compressibility, and microstructural properties of sintered α-alumina samples. Moreover, the effect of compaction pressure on the green density of the compacts is studied by applying different pressures ranging from 400 to 550 MPa. Samples were prepared by mechanical blending of alumina and various amounts of PEG powders in a Turbula mixer. The binder contents vary from 1 wt.% to 4 wt.%. The as-prepared mixture was compacted in a universal machine at room temperature under the pressure of 6 MPa to produce disk-shaped samples in a pre-compaction step. Experimental results revealed that adding various amounts of PEG powders has a detrimental effect on the green density of alumina pellets and decreases the green density from 1.95 to 1.87 g/cm³. The results also show that sintered density of samples increased by increasing the compaction pressure to pressures higher than 400 MPa. It is observed that a sudden increase in green density has been observed between 450 and 550 MPa.     

Dispersion and densification of nano Si–(Al)–C powder with amorphous/nanocrystalline bimodal microstructure

The dispersion behavior and densification of nano Si–(Al)–C powder with amorphous/nanocrystalline bimodal microstructure were investigated. The Si–C powders synthesized by a mechanical alloying (MA) process had a near‐spherical shape with an average particle size of 170 nm. A solid loading of 62 vol% was achieved using polyethyleneimine (PEI) as a dispersant. The optimum dispersant amount was 1 wt% based on zeta potential, sedimentation, and viscosity analysis data. The high zeta potential value (73 mV) compared with that of the commercially available SiC (65 mV) was caused by modified surface properties and consequent promotion of the cationic dispersant adsorption. A Si–Al–C slurry containing 6.5 wt% of sintering additives with a solid loading of 60 vol% was also prepared. The relative density of the dried Si–Al–C slurry was 63.3% without additional compaction, which could be densified at 1650°C at a pressure of 20 MPa using a spark plasma sintering furnace.     

Study of fragmentation in cBN powders under ultra-high pressure

Studying the fragmentation law and refinement of cubic boron nitride powder under ultra-high pressure is crucial to producing a high-strength, high-density polycrystalline cubic boron nitride. In this paper, brown and black cBN crystalline powders with different micron sizes were selected as initial raw materials for an ultra-high-pressure simulation experiment. Single and mixed particles were extruded under 80MPa low pressure and 5.5GPa ultra-high pressure at ambient temperature for 1 min. The crushing behavior and particle size distribution of cBN powders with different particle sizes and ratios were investigated using a laser particle size analyzer and scanning electron microscopy. Results revealed no particle breakage or deformation at low pressure, and the compaction density was low. However, under ultra-high pressure, the cBN particles showed cracks, plastic deformation, and fragmentation, resulting in crushed fine particles filling in the voids of coarse particles, which led to a higher pressing density. Small-sized or mixed cBN particles with high density ratios were not easily crushed; the coarser the particle size, the more severe the ultra-high-pressure extrusion and crushing. The pressing density also declined, and brown cBN crystal particles with higher impact toughness demonstrated a lower particle breakage rate. The ultra-high-pressure crushing law should be considered and appropriate binders should be selected to improve the sintering performance of PcBN materials; ultra-high-pressure crushing of cBN powder contributes to cBN-cBN and cBN-M-cBN bonds under high temperatures and ultra-high pressure.     

Preparation of high-strength Mg-3Al-Zn alloy with ultrafine-grained microstructure by powder metallurgy

Mg-3Al-Zn alloys with ultrafine grain size (UFG) have been fabricated by consolidation of ball milling nanocrystalline powders. Firstly, the elemental powders of Mg, Al and Zn were ball milled to synthesize nanocrystalline alloy powders. The milled powders stored in an Al container were sintered for 40 min at 633 K in a vacuum furnace. The sintered samples were extruded at the temperature range from 373 to 573 K for further densification. The bulk alloys with an average grain size of 180 nm showed a yield stress of 379 MPa, which was two times higher than that of the coarse-grained AZ31, and their ultimate strength was 417 MPa with a 5% elongation. The high strength of the alloys was attributed to three strengthening mechanism: the fine grain strengthening, dispersion strengthening and solid solution strengthening. Low strain hardening was observed in the UFG alloy, which may be caused by room temperature dynamic recovery during plastic deformation.     

Performance evolution of NiO/yttria-stabilized zirconia anodes fabricated at different compaction pressures

Nickel oxide (NiO)/yttria-stabilized zirconia (YSZ) anode substrates were fabricated at four compaction pressures, 70, 200, 500 and 1000 MPa, the particle size distributions of NiO and YSZ were investigated with the powders treated at different compaction pressures, and the effects of compaction pressure on the performance of anodes with and without pore-formers were investigated by studying the effects of compaction pressure on the sintering shrinkage, compaction density, sintered density and electrical conductivity of anodes and the performance of cells. Experimental results demonstrated that the mismatch in the sintering shrinkages of YSZ films and the anodes compacted at 70 and 1000 MPa caused gas leakage across the films and thus a higher local temperature than the furnace temperature. The single cell with the anode using pore-former and compacted at 500 MPa exhibited the best output performance of 2.66 W cm⁻² at 800 °C.     

Effect of the CoFe2O4 initial particle size when sintered by microwave on the microstructural,dielectric, and magnetic properties

The particle size of CoFe₂O₄ powders (average particle size of 350 nm) was reduced to 50 nm by high-energy milling. In this paper, special attention was given for analyzing the densification and grain growth of both particle sizes (350 and 50 nm) subject to ultrafast sintering assays using microwave sintering and their effect on the magnetic and electric properties. The results indicated that the grain growth was 10 times higher for the nanoparticle system, reaching similar sizes of ~1 μm in both cases after sintering. The relative density values were higher (95%) in the nanoparticle system due to the wide distribution of particle sizes generated in the grinding process. Qualitatively inferred microscopy analysis showed high sinterability of fine particles with a narrow distribution of grain size when subjected to ultrafast firing processes. Magnetization measurements at room temperature clearly show the reduction of Hc with increasing grain size. Electric resistivity, dielectric constant (ε′), and dielectric loss tangent (tan δ) were measured as a function of frequency at room temperature. The low values of dielectric constant (ε′) and dielectric loss (tan δ) in the low frequency range, shown for all samples sintered by microwave, prove the excellent uniformity in the microstructure.     

固相烧结——Ⅲ 实验：超细氧化锆素坯烧结过程中的 晶粒与气孔生长及致密化行为

研究了超细Y-TZP和YSZ粉料成型体在烧结中期的晶粒生长、气孔生长和致密化行为.根据作者前文     

Influence of solid loading and particle size distribution on the porosity development of green alumina ceramic mouldings

Alumina ceramic mouldings with different solid contents ranging from 55 to 70 vol% and different ratios of coarse/fine powders, i.e. 0.4 μm (fine) and 3 μm (coarse), respectively, were prepared by compression moulding at 75 °C under a compressive stress of 10 MPa. The porous parameters, such as porosity, pore size and pore size distribution, of the green compacts were evaluated after removal of organic vehicles. Experimental evidence showed that the green density, as well as the sintered density, of the moulded alumina increased linearly with increased solid loading to an optimum of 65 vol% and decreased roughly linearly with increased coarse/fine ratio. Further increase in solid loading reduced particle packing efficiency, resulting in lower green and fired densities. No considerable improvement in green and sintered density of the moulded alumina was achieved by adjusting the coarse/fine ratio, which is due to the fact that coarse particles suppress the driving force of densification. The green compacts generally showed a bimodal pore size distribution character which may be the most important factor in dominating the densification of the powder compacts. The peak frequency at larger pore region is approximately 20–35 μm in diameter and at the smaller pore region is ˜50–95 nm in diameter. The larger pores are believed to be due to the presence of internal voids originating from entrapped gas and are probably caused by the removal of organic vehicles.