Forming and sintering behaviors of commercial α-Al2O3 powders with different particle size distribution and agglomeration

The Al₂O₃ structure ceramics have been investigated extensively in previous studies. In order to compare micron- with submicron-scale powder on forming and sintering behaviors, three commercial α-Al₂O₃ powders were studied: 0.15 μm (denoted S as small in the paper) (granulating), 0.43 μm (denoted M as middle) (granulating), and 1.8 μm (denoted L as large) (granulate-free) at d₅₀ (median size). Although the (M) powder contains hard agglomerates, it forms more easily than the (S) powder. This is principally because the (M)'s soft agglomeration strength (0.03 MPa) is weaker than (S) (7 MPa). The (L) bulk formed easily with lower pressure 10 MPa because of wider starting-particle size distribution, 0.2–15 μm. The (S) primary particles rearranged before sintering, so it postponed its sintering onset temperature to about 1200 °C. Additionally, its shrinkage rate becomes maximal and concentrated at the 2nd stage of sintering from 1300 to 1400 °C. (M) bulk revealed the longest shrinkage range from 1000 to 1500 °C because the sintering occurred with its hard agglomerates at first. Although (L) powder formed rather easily, its sintering was impeded by a much wider particle size distribution.     

The effect of submicron-sized initial tungsten powders on microstructure and properties of infiltrated W-25 wt.% Cu alloys

In the present work, several W-25 wt% Cu alloys have been prepared through combined processes of high-energy ball-milling, liquid-phase sintering and infiltration, using the precursors of industrial copper powders with an average particle size of 50 μm and tungsten powders with alternative average particle size of 8 μm, 800 nm, 600 nm or 400 nm. Microstructure characteristics, relative density, hardness and electrical conductivity of the WCu alloys were investigated to elucidate the effect of initial particle size of tungsten powders. EBSD was further utilized to reveal the orientation and grain size distribution in the WCu alloys prepared by 8 μm and 400 nm-sized tungsten powders. The results showed that the WCu alloy made by 400 nm-sized tungsten powders exhibited excellent homogeneity for both sintered tungsten powders and grains, together with the highest relative density of 98.9%, the highest hardness of 230 HB, and good electrical conductivity of 48.7% IACS. Moreover, it also showed highly improved arc erosion and mechanical wear resistances.     

Effect of initial particulate and sintering temperature on mechanical properties and microstructure of WC–ZrO2–VC ceramic composites

Owing to improving the mechanical properties of cemented carbides in high speed machining fields, a new composite tool material WC–ZrO₂–VC (WZV) is prepared from a mixture of yttria stabilized zirconia (YSZ) and micrometer VC particles by hot-press-sintering in nitrogenous atmosphere. Commercial WC, of which the initial particle sizes are 0.2 μm, 0.4 μm, 0.6 μm and 0.8 μm, is mixed with zirconia and VC powder in aqueous medium by following a ball mill process. The sintering behavior is investigated by isostatic pressing under different sintering temperature. The relative density and bending strength are measured by Archimedes methods and three-point bending mode, respectively. Hardness and fracture toughness are performed by Vickers indentation method. Microstructure of the composite is characterized by scanning electron microscopy (SEM). The correlations between initial particles, densification mechanism, sintering temperature, microstructure and mechanical properties are studied. Experimental results show that maximum densification 99.5% is achieved at 1650 °C and the initial particle size is 0.8 μm. When temperature is 1550 °C and particle size is 0.4 μm, the optimized bending strength (943 MPa) is obtained. The best hardness record is 19.2 GPa when sintering temperature is 1650 and particle size is 0.8 μm. The indention cracks propagate around the grain boundaries and the WC particles fracture, which is associated with particle and microcrack toughening mechanism.     

Microstructure evolution of grey cast iron powder by high pressure gas atomization

The grey cast iron powders were prepared by high pressure gas atomization. Calculation results show that the cooling rates of droplets of grey cast iron reach to 10⁴ to 10⁶ K s^?1 in the experiments. Microstructures of atomized grey cast iron powders with different diameters were characterized by X-ray diffraction, optical microscopy and scanning electron microscopy. Microstructures of powders under 38 μm in diameter are mainly γ-Fe and a little α-Fe. With the increase of powder diameter, content of γ-Fe phase gradually decreases, while content of α-Fe phase increases. When the diameter is over 150 μm, powders are completely composed of α-Fe phase. By measuring the spatial variation in microstructural scales within powders, the results show the lamellar spacing increases with the increase of powder diameter. As the powder size is larger than 106 μm, the increase trend of the lamellar spacing becomes smaller.     

Ceramic processing strategies for thick films on copper foils

Functional oxides on Cu have multiple applications. For thick films the required high sintering temperatures present a challenge for processing on base metal substrates. In this study it is shown that it is possible to adapt well-known ceramic processing strategies to the fabrication of thick lead zirconate titanate (PZT) films on Cu with useful ferroelectric properties. PZT powders with optimized particle sizes are used to fabricate thick films by electrophoretic deposition in combination with a post-deposition isostatic pressing step. This approach to maximize green packing is sufficient to dramatically lower the required sintering temperatures. 25 μm thick PZT films on Cu sintered at 900 °C have a dielectric permittivity of 585, a loss tangent at 10 kHz of 0.03, a remanent polarization of 19 μC cm^?2 and a coercive field of 22 kV cm^?1. This significant improvement in the dielectric response opens the possibility of using thick PZT films on Cu for a wide range of devices where cost, yield and reliability are concerns.     

Formation of porous metallic glass compacts by electro-discharge sintering

A single pulse of 0.1–0.9 kJ/0.45 g atomized amorphous Cu₅₄Zr₂₂Ti₁₈Ni₆ powders in size range of 90–150 μm was applied to fabricate porous metallic glass compacts using electro-discharge sintering (EDS) with 3 and 4 mm in diameter. The structural and thermal analysis of the samples indicated that formation of the porous metallic glass compacts occurs only when low electrical input energy was induced on the amorphous powders. Furthermore, the critical input energy inducing crystallization of the amorphous phase during EDS is strongly dependent on the size of the sample.     

Sintering of tungsten powder with and without tungsten carbide additive by field assisted sintering technology

Tungsten powder (0.6–0.9 μm) was sintered by field assisted sintering technology (FAST) at various processing conditions. The sample sintered with in-situ hydrogen reduction pretreatment and pulsed electric current during heating showed the lowest amount of oxygen. The maximum relative density achieved was 98.5%, which is from the sample sintered at 2000 °C, 85 MPa for 30 min. However, the corresponding sintered grain size was 22.2 μm. To minimize grain growth, nano tungsten carbide powder (0.1–0.2 μm) was used as sintering additive. By mixing 5 and 10 vol.% WC with W powder, densification was enhanced and finer grain size was obtained. Relative density above 99% with grain size around 3 μm was achieved in W–10 vol.% WC sintered at 1700 °C, 85 MPa, for 5 min.     

Thermal explosion synthesis of ZrC particles and their mechanism of formation from Al–Zr–C elemental powders

ZrC particles were fabricated by thermal explosion (TE) from mixture of Al, Zr and C elemental powders. Without the addition of Al, the synthesized ZrC particles had irregular shape of ~ 4.0 μm in average. Increasing Al content up to 30 wt.%, however, refined significantly them down to < 0.2 μm with regularly square morphology. The Al effect of reaction mechanism promoted the ZrC formation as diluents in the course of TE, which was clarified using differential thermal analysis and X-ray diffraction technique. The melting of Al favored the reaction with Zr to generate ZrAl₃, and then the dissolution of C into the Al–Zr liquid resulted in precipitation of ZrC. Meanwhile, the exothermic effect prompted C atoms dissolving into Zr–Al liquid and eventually led to precipitation of ZrC out of the supersaturated liquid. The Al addition inhibited particle growth, but also promoted the TE reaction.     

Preparation of spherical silica powder by oxygen–acetylene flame spheroidization process

A novel economic oxygen–acetylene flame spheroidization process and special equipments to prepare spherical silica powders are presented. Before spheroidization treatment, the raw silica is purified by mixed acids. In this spheroidization process, oxygen is used both as the carrier gas to transport the purified silica powders to the flame region, and as the combustion-supporting gas. The crystallized silica powders are melted and then transformed to amorphous silica after oxygen–acetylene flame spheroidization treatment. The powder size analysis indicates that the powder size increases and the size distribution become narrower after spheroidization treatment. By optimizing the process parameters, spherical silica powders were obtained. A scanning electron microscope (SEM) investigation reveals that the spheroidization efficiency of the 5 μm diameter powder is more than 95% at feeding rates below 60 g/min. The closer the length–diameter ratio of raw silica powder is to 1, the higher the spheroidization efficiency of the sample is. The fluidity value and apparent density of the powder with the spheroidization efficiency 95% is 70 s/50 g and 0.88 g/cm³, respectively. Oxygen–acetylene flame spheroidization process is a promising low-cost alternative for large-scale production of spherical silica powder.     

Preparation of ultra fine copper–nickel bimetallic powders for conductive thick film

In this paper, ultrafine nickel-rich Cu–Ni bimetallic powders were synthesized with hydrothermal-reduction method. When polyethyleneglycol (PEG) was employed as protective agent, flake bimetallic powder particles, which have an excellent dispersibility and uniform size of 1.8–2.0 μm, can be prepared. Polyhedral powder particles, which have a uniform particle size in the range from 0.5 to 0.8 μm, were successfully synthesized using gelatin as protective agent. By thermal analysis, it was found that the oxidation-resistance of Cu–Ni powder particles was strong. Above-mentioned flake/polyhedral bimetallic powders were mixed with inorganic binder and vehicle to make conductive thick film. The low resistivity and high adhesion strength of thick film were attributed to high densification and rough interface from interfacial reaction, respectively.     

The effects of ball-milling treatment on the densification behavior of ultra-fine tungsten powder

Ultra-fine tungsten powder with a BET particle size of 210 nm was synthesized by sol spray drying, calcination and subsequent hydrogen reduction process. Then this powder was treated by ball-milling, the characteristic changes of this powder before and after milling were investigated. Then the sintering densification behavior of these powders with different ball-milling time (0 h, 5 h, 10 h) were also studied. The results show that ball-milling treatment greatly activates the sintering process of ultra-fine tungsten powder. The relative density of the powder ball-milled for 10 h could reach 97.3% of theoretical density (TD) when sintered at 1900 °C for 2 h, which is 600 °C lower than the required temperature of the traditional micro-scaled powder sintered for the same density. At the same time, ball-milling treatment could substantially reduce the onset temperature of sintering as well as recrystallization, and bulk tungsten materials with more uniform and finer microstructure and much better mechanical properties (hardness) could be obtained.     

Application of compression lubricant as final porosity controller in the sintering of tungsten powders

Sintering behavior of two tungsten powders (1.2 μm and 6 μm) was studied for preparing infiltrable porous skeleton. Both powders were compressed by mechanical press (MP) and cold isostatic press (CIP) with and without stearic acid respectively as compaction lubricant. Results showed that presence of solid lubricant powder in addition of its essential effect on soundness of parts, depending on its size and distribution, could mainly affect sintered microstructure. Stearic acid as compaction lubricant in addition of decreasing friction between particles during the compaction, has acted as spacing particles between primary powder particles. In the cases that lubricant particles are much bigger than tungsten particles a big pore remained after evaporation of lubricant. During the sintering, big pores became bigger due to coarsening mechanism and formed an interconnected network of pores and on the other hand small pores shrank or even disappeared due to densification. By exact controlling of the size of tungsten powder and lubricant powder, infiltrable tungsten skeletons with 80% of theoretical density were produced successfully at low sintering temperatures such as 1500 °C.     

Nano-sized zirconium carbide powder: Synthesis and densification using a spark plasma sintering apparatus

Nano-sized zirconium carbide powder was synthesized at 1600 °C by the carbothermal reduction of ZrO₂ using a modified spark plasma sintering (SPS) apparatus. The synthesized ZrC powder had a fine particle size of approximately 189 nm and a low oxygen content of 0.88 wt%. The metal basis purity of the synthesized powder was 99.87%. The low synthesis temperature, fast heating/cooling rate and the effect of current during the modified SPS process effectively suppressed the particle growth. Using the synthesized powder, monolithic ZrC ceramics with high relative density (97.14%) were obtained after the densification at 2100 °C for 30 min at a pressure of 80 MPa by SPS. The average grain size of the densified ZrC ceramics was approximately 9.12 μm.     

Effect of powder mixing on thermoelectric properties in Bi2Te3-based sintered compounds

The effect of powder mixing on thermoelectric properties was studied in n-type Bi₂Te_2.85Se_0.15 compounds and p-type Bi_0.5Sb_1.5Te₃ compounds. The figure-of-merit of the n- and p-type sintered compounds was strongly affected by carrier mobility. The use of coarse powders (200–300 μm) was beneficial to improve the crystallographic orientation of sintered compound. However, voids in the compound decreased the carrier mobility. As the fine powders (below 45 μm) were blended with coarse powders up to about 30%, the carrier mobility was increased due to the reduction of the voids. The addition of fine powders over 30% degraded the carrier mobility due to the decrease of crystallographic orientation and the increase of particle boundary. When the fine powder content was 20%, the n- and p-type compounds exhibited the maximum figure-of-merit of 2.31 × 10⁻³ K⁻¹ and 2.89 × 10⁻³ K⁻¹, respectively.     

High-temperature strength of compacted sub-micrometer aluminium powder

Aluminium powders with a mean particle size of around 1 μm were compacted by cold isostatic pressing (CIP) and additional forging. The specimens are characterized by hot compression tests, dilatometry and metallography. A 3D interconnected structure of alumina films <5 nm in thickness is observed by transmission electron microscopy and field emission gun scanning electron microscopy; it is associated with the natural oxide skin which covers every aluminium powder and occupies around 3 vol.%. The compression tests are carried out in the range of 350–520 °C at strain rates of 0.003–3 s^?1. The compressive strength was 100–150 and 130–180 MPa for the CIPed and forged samples, respectively. The low strain rate sensitivity m (<0.08) suggests that the alumina network forms a barrier, which suppresses any restoration mechanism across the grain boundaries as well as grain boundary sliding during hot deformation. The high strength of such compacted sub-micron Al powder is attributed to the conservation of a 3D alumina closed cell network filled with elastoplastic aluminium.     

Self-compacting high density tungsten–bronze composites

Green compacts of W–bronze were encapsulated in shells of bronze powder, placed in a ceramic mold and sintered in alumina tube furnace at 1150 °C. Throughout the sintering cooling stage the differential coefficient of thermal expansion ΔCTE of W–bronze was employed to induce an external compressive densification action. The process included simultaneous sintering, hot isostatic pressing (HIP) and infiltration act to enhance densification. By this technique, pilot sintered compacts of different W50–80 wt.%–pre-mix bronze of 97–99% theoretical density were produced. This process resulted in compacts of higher hardness, higher sintered density and better structure homogeneity as opposed to similar compacts densified by the conventional sintering process. The results showed a gain in hardness by 10–20% and in density by 5–15%. The impact of different cooling rates of 3, 4, 8 and 30 °C min^?1 on sintered density, microstructure and densification mechanisms was examined and evaluated. Low cooling rates of 3 and 4 °C min^?1 gave the best results.     

Synthesis of nanosized composite powders via a wet chemical process for sintering high performance W-Y2O3 alloy

With the aim of preparing high performance oxide dispersion strengthened tungsten-based alloys by powder metallurgy, the W-Y₂O₃ composite nanopowders were prepared by an improved bottom-up wet chemical method. Ultrasonic treatment and anionic surfactant sodium dodecyl sulfate (SDS) addition were innovatively introduced into this wet chemical method in order to fabricate homogeneous, ultrafine W-Y₂O₃ composite nanopowders. As a result, the average tungsten grain size of 40–50 nm was obtained for this composite nanopowders. For comparison, W-Y₂O₃ composite powders were also prepared by traditional mechanical milling. After that, spark plasma sintering (SPS) was employed to consolidate the powders prepared by either mechanical milling or wet chemical method to yield high density as well as suppress grain growth. It is found that the W-Y₂O₃ alloy prepared by wet chemical method and subsequent SPS possesses smaller grain size (0.76 ± 0.17 μm) and higher relative density (99.0%) than that prepared by mechanical milling and subsequent SPS. Moreover, the oxide nanoparticles (about 2–10 nm) are dispersed within tungsten grains and at grain boundaries more uniformly in W-Y₂O₃ alloy prepared by wet chemical method and subsequent SPS. Due to the ultrafine grains, high sintering density and homogeneously distributed oxide nanoparticles, the Vickers microhardness of yttria dispersion strengthened tungsten-based alloy prepared in our work reaches up to 598.7 ± 7.3 HV_0.2, higher than that reported in the previous studies. These results indicate that the improved bottom-up wet chemical method combined with ultrasonic treatment and anionic surfactant addition developed in our work is a promising way to fabricate high performance oxide dispersion strengthened tungsten-based alloys with ultrafine grain and high density.     

Properties of Pb(Zr, Ti)O3 fibres with a radial gradient structure

One difficulty during the fabrication of lead zirconate titanate (PZT) materials is the high partial pressure and the accompanied evaporation of lead oxide (PbO) during sintering. To overcome this problem, atmospheric powders are used in the sintering step, whereby a composition and microstructure gradient across the fibre radius can be expected. In this study, therefore, the microstructure (porosity, grain size), the chemical and the phase composition as well as the ferroelectric properties were analysed across the fibre diameter. For these investigations, extruded PZT fibres with a green diameter of 300 μm and 70 μm were sintered at 1200 °C for 2 h in a PbO-enriched atmosphere. The measurements revealed that the chemical and thus the phase composition vary across the radius of the fibres for both fibre diameters, but the observed gradients are much more pronounced for 70 μm fibres. By removing the affected surface layer of a 300 μm diameter fibre, the maximum free strain could be increased by 20%.     

Effect of ball-milling time on structural characteristics and densification behavior of W-Cu composite powder produced from WO3-CuO powder mixtures

Understanding the microstructure of W–Cu nanocomposite powder is essential for elucidating its sintering mechanism. In this study, the effect of milling time on the structural characteristics and densification behavior of W-Cu composite powders synthesized from WO₃-CuO powder mixtures was investigated. The mixture of WO₃ and CuO powders was ball-milled in a bead mill for 1 h and 10 h followed by reduction by heat-treating the mixture at 800 °C in H₂ atmosphere with a heating rate of 2 °C/min to produce W-Cu composite powder. The microstructure analysis of the reduced powder obtained by milling for 1 h revealed the formation of W–Cu powder consisting of W nanoparticle-attached Cu microparticles. However, Cu-coated W nanocomposite powder consisting of W nanoparticles coated with a Cu layer was formed when the mixture was milled for 10 h. Cu-coated W nanopowder exhibited an excellent sinterability not only in the solid-phase sintering stage (SPS) but also in the liquid-phase sintering stage (LPS). A high relative sintered density of 96.0% was obtained at 1050 °C with a full densification occurring on sintering the sample at 1100 °C. The 1 h-milled W-Cu powder exhibited a high sinterability only in the LPS stage to achieve a nearly full densification at 1200 °C.     

Structural and mechanical characteristics of porous 316L stainless steel fabricated by indirect selective laser sintering

Selective laser sintering (SLS) technique is capable of rapidly fabricating customized implants with porous structure. A simple encapsulation process was developed to coat 316L stainless steel (316L SS) powder with ethylene-vinyl acetate copolymer (EVA). Subsequently, porous 316L SS was prepared by SLS preforming of EVA-coated metal powders, debinding and sintering in hydrogen atmosphere. The effects of processing parameters on pore characteristics and mechanical properties were analyzed. The results indicate that the porosity of green body mainly depends on laser energy density, while the pore features and mechanical properties of sintered specimens are largely dominated by sintering temperature. After sintering at 1100–1300 °C, the average pore size and porosity are 160–35 μm and 58–28%, respectively. In addition, the elastic modulus and compressive yield strength are 1.58–6.64 GPa and 15.5–52.8 MPa, respectively. It is revealed that the pore structural parameters and mechanical properties of the as-sintered porous 316L SS can be controlled readily to match with those of cancellous bone by modification of SLS processing parameters and subsequent sintering temperature.