Sintering of Mixtures of Seeded Boehmite and Ultrafine α-Alumina

α-Alumina was fabricated by dry pressing mixtures of seeded boehmite and fine α-alumina (i.e., 0.2 and 0.3 μm diameter) to reduce the large shrinkage of boehmite-derived α-alumina. The maximum green density was obtained with mixtures containing ∼70%α-alumina for both alumina powders. The ∼15% linear shrinkage and microstructures of these samples were comparable to 100% alumina powder samples. Samples with 0.2 μm alumina sintered to densities >95% at 1300°C whereas 1400°C was needed for samples with 0.3 μm alumina. These results indicate that boehmite can be used as a substitute for relatively expensive ultrafine α-alumina powders.     

Low-temperature sintering of single-phase,high-entropy carbide ceramics

Dense (Hf, Zr, Ti, Ta, Nb)C high-entropy ceramics were produced by hot pressing (HP) of carbide powders synthesized by carbothermal reduction (CTR). The relative density increased from 95% to 99.3% as the HP temperature increased from 1750°C to 1900°C. Nominally phase pure ceramics with the rock salt structure had grain sizes ranging from 0.6 µm to 1.2 µm. The mixed carbide powders were synthesized by high-energy ball milling (HEBM) followed by CTR at 1600°C, which resulted in an average particle size of ~100 nm and an oxygen content of 0.8 wt%. Low sintering temperature, high relative densities, and fine grain sizes were achieved through the use of synthesized powders. These are the first reported results for low-temperature densification and fine microstructure of high-entropy carbide ceramics.     

Single-step,high pressure,and two-step spark plasma sintering of UO2 nanopowders

Three different spark plasma sintering (SPS) treatments were applied to highly sinteractive, near-stoichiometric UO_2.04 nanocrystalline (5 nm) powders produced by U(IV) oxalate hydrothermal decomposition at 170 °C. The sintering conditions for reaching 95 % theoretical density (TD) in regular SPS, high pressure SPS (HP-SPS), and, for the first time, two-step SPS (2S-SPS), were determined. Densification to 95 % TD was achieved at 1000 °C in regular SPS (70 MPa applied pressure), 660 °C in HP-SPS (500 MPa), and 650?550 °C in 2S-SPS (70 MPa). With the goal of minimising the grain growth during densification, the sintering treatments were optimised to favour densification over coarsening, and the final microstructures thus obtained are compared. Equally dense UO₂ samples of different grain sizes, ranging from 3.08 μm to 163 nm, were produced. Room-temperature oxidation of the powders could not be avoided due to their nanometric dimensions, and a final annealing treatment was designed to reduce hyperstoichiometric samples to UO_2.00.     

Low temperature sintering of PZT powders coated with Pb5Ge3O11 by sol–Gel method

Low temperature sintering of PZT powders was investigated using Pb₅Ge₃O₁₁(PGO) as a sintering aid. PZT powders with 150 nm particle size were coated with PGO which was prepared from precursor solutions of Ge(OiPr)₄ and Pb(NO₃)₂ by sol–gel method. 1 wt% PGO-added PZT powders were densified at 750°C for 2 h to sintered bodies with the relative density of approximately 95%. An addition of PGO improved the sinterability of PZT powders with a reduction of sintering temperature by about 300°C. Dielectric and piezoelectric properties of PGO-added PZT ceramics sintered at ≦950°C were superior to those without PGO additives. However, a higher sintering temperature above 1000°C deteriorated the dielectric and piezoelectric properties of PGO-added PZT ceramics. This may be attributed to the change of microstructure involving the formation of solid solution between PZT and PGO. The 1 wt% PGO-added PZT bodies sintered at 750°C exhibited an electromechanical coupling factor, Kp, of about 56%.     

Effect of Co-Precipitation on the Low-Temperature Sintering of Biphasic Calcium Phosphate

Three types of biphasic calcium phosphate (BCP) powders were prepared and their sintering behavior was investigated. The specific surface area and HA/TCP ratio were similar in all three specimens. Most of the densification in the co-precipitated s-BCP occurred before the β- to α-TCP phase transformation, and a maximum density of ∼95% was obtained at 1100°C. The mixture of separately precipitated and calcined hydroxyapatite (HA) and tricalcium phosphate (TCP) (m-BCP) showed a poor sintering behavior, and the apparent density was below 70% at temperatures up to 1200°C. In the commercial HA and TCP mixture (c-BCP), the low temperature sintering was poor, but densification continued without the phase transformation due to the presence of MgO, achieving almost full densification at 1200°C.     

Synthesis and Sintering Behavior of Ultrafine (<10 nm) Magnesium Aluminate Spinel Nanoparticles

This article reports a comparative characterization of ultrafine MgAl₂O₄ spinel nanoparticles synthesized by polymeric precursor (Pechini) and coprecipitation methods. The nanoparticles were evaluated in terms of purity and surface cleanliness, size distribution, state of agglomeration, and sintering behavior. Powders synthesized by the Pechini technique were highly agglomerated and revealed a bimodal particle size distribution centered around 12 and 27 nm. Thermal analysis and infrared spectroscopy measurements indicated that carbon species remained on the surface of the powders only to be released when temperatures exceeded 1000°C. Isothermal sintering of such nanopowders at 1300°C showed a maximum relative density of only 54%. MgAl₂O₄ synthesized via coprecipitation created small nanoparticles, around 5–6 nm after calcination at 800°C, with significantly less agglomeration. Compared with the precursor‐derived powders, excellent sinterability of the coprecipitated powders was obtained under the same sintering conditions. Relative densities above 90% were obtained after only 10 min, which further increased to greater than 95% after 20 min with no sintering aids or dopants. The results highlight the importance of purity and processing control to exploit the beneficial high sinterability of nanoparticles.     

Porous Pb(Zr0.95Ti0.05)O3 Ceramics from Chemically Prepared Powders Without Pore Formers

Porous Zr-rich lead zirconate titanate (PZT 95/5) ceramics having 77.9–92.2% of relative densities were prepared without additional pore formers. PZT 95/5 powders were obtained by a one-step pyrolysis process at 450°C for 10 h using the Pechini method. Although the X-ray diffractometry results showed an incomplete perovskite phase for the powders, phase-pure PZT 95/5 ceramics could be obtained after sintering at 1100°–1150°C for 2 h. The density and diameter variations of the PZT 95/5 ceramics as a function of sintering temperature were investigated.     

New Methods for Preparing Submicrometer Powders of The Tungstate‐Ion Conductor Sc2(WO4)3 and its Al and In Analogs

Two new methods for preparing submicrometer powders of M₂(WO₄)₃, M = Sc, In, and Al via combustion synthesis are reported. Stoichiometric combinations of trivalent metal nitrates, ammonium metatungstate, and either urea or carbohydrazide as the fuel were reacted at 550°C, producing amorphous or poorly crystallized powders with an average particle size ranging from 164 to 350 nm. Calcining the powders at 800°C for 1 h produced well‐crystallized, phase‐pure powders with an average particle size ranging from 210 to 711 nm. Powders sintered at 1000°C for 14 h resulted in pellets that were 87%–95% of the theoretical density, which is notably higher than typically obtained from powders prepared by solid‐state reaction. Whereas there was little difference in the microstructure of Al₂(WO₄)₃ pellets prepared with the two different powders, the carbohydrazide‐derived powders resulted in In₂(WO₄)₃ and Sc₂(WO₄)₃ pellets with a larger grain size than those prepared with urea‐derived powders. The electrical conductivity of the sintered pellets, while comparable to that reported for polycrystalline M₂(WO₄)₃ prepared by solid‐state reaction, was strongly influenced by grain‐boundary effects.     

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.     

Densification of Sol-Gel-Derived Mullite Ceramics after Cold Isostatic Pressing up to 1 GPa

Molecular-designed ultrafine mullite precursor powders with a stoichiometric composition were prepared by copolymerization of alkoxides. The precursor powders were calcined in the range from 800° to 1200°C and consolidated by ultra-high-pressure cold isostatic pressing up to 1 GPa. Ultrahigh isostatic pressure of 1 GPa led to a closed packing structure in the green compacts. Interaggregate pores in the green compacts were collapsed by the ultrahigh cold isostatic pressure to reduce the pore size below 6 nm. As a result, the maximum density of the green compacts reached 70% of theoretical. These closely packed green compacts of precursor powders with a stoichiometric composition and calcined at relatively low temperatures could be sintered to >95% of theoretical at 1500°C. Relatively low-temperature sintering below the liquid formation temperature resulted in fine microstructure of the resultant mullite ceramic with a grain size below 300 nm.     

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.     

Mechanical properties of in situ synthesized mullite-based composite ceramics with three-dimensional network structure

Needle-like nanocrystalline mullite powders were prepared through the molten salt process at the temperature of 900°C using coal gangue as raw material. Then, mullite-based composite ceramics were prepared by a conventional solid-state reaction between in situ synthesized mullite and Al₂O₃ powders. Effects of Al₂O₃ content and sintering temperatures on phase compositions, microstructure, and mechanical properties of the mullite-based composite ceramics were also studied. The results show that mullite content productivity increase from 72% to 95%, as the sintering temperature increased from 1480°C to 1580°C, which led to the improvement in the bulk density and flexural strength of the samples. The three-dimensional interlocking structure for mullite-based composite ceramics was obtained by the in situ solid-state reaction process. The maximum bulk density, flexural strength, and fracture toughness for the sample with 15 wt% Al₂O₃ content are 2.48 g/cm³, 139.79 MPa, and 5.62 MPa··m^1/2, respectively, as it was sintered at the temperature of 1560°C for 3 h. The improved mechanical properties of mullite-based composite ceramics maybe ascribed to good densification and increased mullite phase content, as well as to the in situ three-dimensional network structure. Therefore, the results would provide new ideas for high-value utilization of coal gangue.     

自蔓延低温燃烧-溶胶凝胶合成Ce0.8Sm0.2O1.9及烧结性能

用甘氨酸作还原剂、硝酸盐作氧化剂,采用溶胶-凝胶与自蔓延低温燃烧相结合的方法制备了超细Ce_0.8Sm_0.2O_1.9 (SDC)固溶体,对所合成的粉体分别采用XRD、SEM和BET法进行了表征。结果表明,600℃焙烧产物是具有较高相纯度的单一立方相萤石型结构固溶体,根据XRD估算晶粒度为13～30 nm。甘氨酸与金属硝酸盐(G/N)摩尔比对粉体的微观形貌和烧结性能有很大影响, 当G/N相似文献   

Formation of Lead Zirconate Titanate Powders by Spray Pyrolysis

Twin-fluid atomization spray pyrolysis (SP) has been investigated for the production of lead zirconate titanate (PZT) powders, using aqueous solutions of lead acetate and zirconium and titanium alkoxide precursor reagents. The particle size distribution of the PZT powder showed a d ₅₀ value of 0.3 μm, but with a small fraction of relatively large particles, several micrometers in size. Most particles were spherical but many of the largest particles, in the size range ca. 1–5 μm, were irregular. It was demonstrated that the morphology of the final PZT powder was controlled by decomposition processes occurring during the initial drying stages, at ≤200°C. A pyrochlore or fluorite-type intermediate crystalline phase was present in the final powders, but when the maximum reactor temperature was raised, and/or when the levels of excess lead in the starting solutions were increased, the proportion of the desired perovskite phase increased. However, at the highest process temperatures studied, ∼900°C, small crystallites of another phase formed on the surface of the PZT particles; these were probably lead oxide carbonate particles. Overall, a starting solution composition containing around 5 mol% excess Pb, and a maximum reactor temperature of 800°C, were selected as offering the most suitable conditions for producing PZT (52/48) powder, with minimal secondary phases(s). Preliminary densification studies showed that the powders could be sintered at 1150°–1200°C to give pellets of 95%–96% theoretical density.     

热压烧结制备高密度ZrB2陶瓷

在烧结温度和压力为1950℃和50MPa条件下,分别对ZrB2的原始粉末、球磨粉末、加助烧剂的粉末以及既加助烧剂又进行球磨的粉末进行热压烧结实验。采用阿基米德排水法测出了ZrB2陶瓷的密度;利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、能谱(EDS)等手段对粉体和烧结产物的物相、形貌以及成分进行了表征。结果表明:球磨且加助烧剂镍的粉体烧结所得样品致密性最好,相对密度为99.375%,接近全致密;球磨细粉烧结所得样品次之,相对密度为99.09%;添加助烧剂粉末烧结所得样品相对密度为91.45%;用原始粉末烧结所得样品致密性最差,相对密度为84.7%。采用排水法所测得密度结果与扫描电镜观察所得致密性情况一致。     

Microstructure and Humidity-Sensitive Characteristics of α-Fe2O3 Ceramic Sensor

The microstructure and humidity-sensitive characteristics of α -Fe₂O₃ porous ceramic were investigated. Microporous α -Fe₂O₃ powders were obtained by controlling the topotactic decomposition reaction of α -FeOOH. Water vapor adsorption thermogravimetrical experiments were carried out in the relative humidity (rh) range 0% to 95% on the α -Fe₂O₃ powder and the 900°C sintered compact. The microstructure was investigated by SEM, TEM, Hg intrusion, and N₂ adsorption porosimetry techniques. The humidity sensitivity was investigated by the impedance measurements technique in 0% to 95% rh on the compacts sintered at 50°C steps in the 850° to 1100°C range. Humidity response was found to be affected by the microstructure, i.e., the characteristics of the precursor powders and sintering temperatures.     

Comparison of AC to DC current sources for field-assisted sintering of aluminum alloy 5083 powder

The viability of resistively sintering aluminum 5083 powder with an alternating current (AC) was explored under both as-atomized and cryomilled conditions. Samples were processed under an AC field and a direct current (DC) field. Samples processed by both methods exhibited similar microstructures and densities at different die wall temperatures. For as-atomized powders, similar densities (99% of theoretical [TD]) were achieved at die wall temperatures of 564°C under DC fields and 525°C under AC fields. For cryomilled 5083, densities up to 90% of theoretical were achieved at 550°C under DC fields, while density values 99% of TD were achieved at 500°C under AC fields. Based on these findings, it has been determined that AC fields can be used as an alternative to SPS for achieving optimal density.     

Comparison of different alumina powders for the aqueous processing and pressureless sintering of Al2O3–SiC nanocomposites

Four different alumina powders, from European and Japanese sources having similar particle size (350–700 nm) were used for the fabrication of nanocomposites. They were compared in terms of green properties, sintering behaviour, microstructure and mechanical properties. The processing route used (attrition milling and freeze-drying) leads to a reduction in green density of the processed aluminas and composites compared to the as-received alumina. All powders had similar green properties except one, which contained a binder from the manufacturer. The presence of this binder led to the formation of hard agglomerates. In this case the pressing did not eliminate, totally, the inter-agglomerate pores, leading to an incomplete sintering. Calcining the powder to remove the binder resulted in similar pressing and sintering behaviour to the other powders and densities >99% were achieved at 1750 °C by pressureless sintering. All the composites exhibited similar microstructures (matrix grain size ∼3 μm) and elastic properties, hardness and fracture toughness. A finer matrix microstructure could be obtained with one of the European powders which achieved ∼99% density at 1700 °C. The presence of 5 vol.% SiC resulted in a mean grain size of ∼2 μm for the alumina matrix compared with 13.9 μm for a monolithic alumina prepared under identical conditions.     

Preparation of nano-AlN powder by sol–gel foaming and its sintering properties

Uniformly dispersed nano-sized aluminum nitride powders were prepared by the sol–gel foaming method using aluminum nitrate as the aluminum source, sucrose as the carbon source, and ammonium chloride as the foaming agent. The effects of ammonium chloride content on the particle size and the sintering properties of aluminum nitride were investigated. The results showed that when the molar ratio of ammonium chloride to aluminum nitrate was .5, the colloidal foams were uniform, large, and fluffy, and amorphous alumina precursors with uniform particles could be prepared. Aluminum nitride powder with a particle size of 22–27 nm can be obtained by calcining these precursors in nitrogen atmosphere at 1400°C for 2 h. At the same time, aluminum nitride bulk material with a relative density of 95% can be obtained by sintering the compact samples in nitrogen atmosphere at 1700°C for 2 h.     

Chemical Synthesis,Sintering and Piezoelectric Properties of Ba0.85Ca0.15 Zr0.1Ti0.9O3 Lead‐Free Ceramics

The preparation of Ba_0.85Ca_0.15 Zr_0.1Ti_0.9O₃ (BCZT) powders by wet chemical methods has been investigated, and the powders used to explore relationships between the microstructure and piezoelectric properties (d₃₃ coefficient) of sintered BCZT ceramics. Sol–gel synthesis has been shown to be a successful method for the preparation of BCZT nanopowders with a pure tetragonal perovskite phase structure, specific surface area up to 21.8 m²/g and a mean particle size of 48 nm. These powders were suitable for the fabrication of dense BCZT ceramics with fine‐grain microstructures. The ceramics with the highest density of 95% theoretical density (TD) and grain size of 1.3 μm were prepared by uniaxial pressing followed by a two‐step sintering approach which contributed to the refinement of the BCTZ microstructure. A decrease in the grain size to 0.8–0.9 μm was achieved when samples were prepared using cold isostatic pressing. Using various sintering schedules, BCZT ceramics with broad range of grain sizes (0.8–60.5 μm) were prepared. The highest d₃₃ = 410.8 ± 13.2 pC/N was exhibited by ceramics prepared from sol–gel powder sintered at 1425°C, with the relative density of 89.6%TD and grain size of 36 μm.