Properties of NiFe2O4 ceramics from powders obtained by auto-combustion synthesis with different fuels

Nickel ferrite (NiFe₂O₄) powders derived by auto-combustion synthesis using three different fuels (citric acid, glycine and dl-alanine) have been characterized. The sintering behavior of ceramics using these powders has been compared. Oxygen balance (OB) setting for the chemical reaction is found to regulate the combustion reaction rate. A rapid reaction rate and a high flame temperature are achieved with dl alanine fuel yielding single phase NiFe₂O₄ powder in the as-burnt stage, whereas powders derived with citric acid and glycine fuels show poor crystallinity and necessitate post-annealing. The powder particles are largely agglomerated with a non-uniform distribution in shape and size, and the average particle size is estimated in the range ~ 54–71 nm. Powders derived from dl-alanine fuel show better phase purity, smaller crystallite size, larger surface area and superior sintering behavior. Additional Raman modes discerned for dl-alanine derived powder support a 1:1 ordering of Ni²⁺ and Fe³⁺ at the octahedral sites relating to microscopic tetragonal P4₁22 symmetry expected theoretically for the formation of NiFe₂O₄ with inverse spinel structure. Microstructure of sintered ceramics depends on the precursor powders that are used and sintering at 1200 °C is found to be optimum. Citric acid and glycine derived powders yield high saturation magnetization (M_s~47–49 emu/g), but poor dielectric properties, whereas dl-alanine derived powders yield ceramics with high resistivity (~3.4×10⁸ Ω cm), low dielectric loss (tan δ~0.003 at 1 MHz) and high magnetization (46 emu/g). Dielectric dispersion and impedance analysis show good correlation with the changes in the ceramic microstructure.     

Synthesis of TiO2–Ag nanocomposite with sol–gel method and investigation of its antibacterial activity against E. coli

TiO₂–Ag nanocomposite was prepared by the sol–gel method and an azeotropic distillation with benzene was used for dehydration of the gel. Because of gel dehydration by distillation method a nanopowder with a surface area of 230 m²/g was produced which decreased to 80 m²/g after calcination. TEM micrographs and XRD patterns showed that spherical nanosized Ag particles (≈ 10 nm) were deposited among TiO₂ particles. The antibacterial activity of calcined powder at 300 and 500 °C was studied in the presence and in the absence of UV irradiation against Escherichia coli as a model for Gram-negative bacteria. The antibacterial tests confirmed the powder calcined at 300 °C possessed more antibacterial activity than the pure TiO₂, amorphous powder and the powder calcined at 500 °C under UV irradiation. In the absence of UV, the reduction in viable cells was observed only with calcinated powder at 300 °C.     

Ba0.6Sr0.4TiO3–MgO ceramics from ceramic powders prepared by improved aqueous gelcasting-assisted solid-state method

Based on aqueous gelcasting-assisted solid-state method (AGASSM), improved aqueous gelcasting-assisted solid-state method (IAGASSM) was proposed to prepare the 45 wt% Ba_0.6Sr_0.4TiO₃–55 wt% MgO (BSTM) ceramic powders. It is found that the BSTM ceramic powders prepared by IAGASSM are the most uniform with the smallest particles (D_av = 0.83 μm) than those prepared by solid-state method (SSM) and AGASSM. The phase compositions of the BSTM ceramic powders and ceramics from the prepared ceramic powders are the same whatever ceramic powder preparation method is adopted. Compared with SSM and AGASSM, the BSTM green samples and ceramics from ceramic powders prepared by IAGASSM are the most uniform. Furthermore, it is found that adopting IAGASSM to prepare ceramic powders could not only improve the dielectric properties of the BSTM ceramics considerably, but also decrease their sintering temperature.     

Particle shape modification and related property improvements

The increasing sophistication of powder metallurgy processing, together with the greater demands on final product quality have led to an increased demand for metal powders of high quality. In this paper we report the successful preparation of two spheroidized metal powders, —electrolytic copper powder mixed with Al₂O₃ particles and hydrogenation-dehydrogenation (HDH) titanium powder — produced by high speed impact using a particle composite system (PCS). Experimental results show that irregularly shaped metal particles can be processed into spherical particles by use of this process. The spheroidizing process increases bulk density of Ti powder from 1.15 g/cm³ to 1.73 g/cm³ and its fluidity index from 46 to 71, improves surface morphology of either single Ti particles or composite Al₂O₃/Cu particles and molding properties of bulk powders. The characteristics of sintered parts made from spheroidized powders are superior to those of products made from the untreated irregular powders.     

Effects of ZrO2 nanoparticles on the microstructure and mechanical properties of ZrO2/AlSi10Mg composites manufactured by laser powder bed fusion

In this work, the nano-ZrO₂ particles were mixed into AlSi10Mg alloy to prepare ZrO₂/AlSi10Mg composites with different x wt.% ZrO₂ (x = 0, 0.15, 0.3, 0.45, 0.6, 0.75). The microstructure, mechanical properties and the anisotropy of the ZrO₂/AlSi10Mg composites fabricated by laser powder bed fusion (LPBF) were studied. The results show that nano-ZrO₂ particles can be uniformly dispersed on the AlSi10Mg powder by the method of pre-dispersion and mechanical mixing. When the mass ratio of ZrO₂ in ZrO₂/AlSi10Mg composites is 0.3 wt%, the values of the tensile strength, yield strength and elongation are 493.64 MPa, 321.30 MPa and 11.74%, respectively. Compared with AlSi10Mg alloy, the tensile strength of ZrO₂/AlSi10Mg composites with 0.3 wt% is increased by 30–55 MPa and the elongation is increased by 3–5%. In addition, the mechanical properties of AlSi10Mg alloy and ZrO₂/AlSi10Mg composites of 0.3 wt% exhibit antistrophic behavior in different direction, which is due to the differences of microstructure, texture and stress distribution between transverse direction (TD) and build direction (BD). Compared with other AlSi10Mg matrix composites, ZrO₂/AlSi10Mg composites of this work show excellent strength and plasticity matching.     

Preparation and magnetoelectric properties of NiFe2O4–PZT composites obtained in-situ by gel-combustion method

Magnetoelectric composites of xNiFe₂O₄–(1 ? x)Pb(Zr,Ti)O₃ with x = 2, 5, 10, 20, 30% were prepared by citrate–nitrate combustion using PZT-based template powders. In order to ensure a better connectivity of dissimilar phases, we have used chemical methods for preparation in situ composites, followed by adequate sintering procedure. The structural, microstructural and functional properties of di-phase magnetoelectric composites of NiFe₂O₄–PZT are reported. The XRD analysis is demonstrating the synthesis of pure ferrite phase directly on the ferroelectric templates. An excellent mixing was obtained in the composite powders, as proved by a detailed SEM analysis.The magnetic and dielectric behaviors of the ceramic composites vary with the ratio of the two phases. The dielectric behavior is greatly influenced by the magnetic phase. The magnetoelectric (ME) coefficient was measured as a function of applied DC magnetic field. The maximum ME coefficient (dE/dH) varies from 0.0011 mV/(cm Oe) to 0.5 mV/(cm Oe) with increasing of NF addition.     

Impact of synthesis method on the properties of near-infrared region-reflective SrSn0.9Mn0.1O3 brown pigment

Brown near-infrared region (NIR) reflective pigment of SrSn_0.9Mn_0.1O₃ was prepared using four different methods: the classical ceramic method, both wet and dry mechanochemical activation processes and the precipitation method. The pigments were characterised in terms of colour properties, NIR reflectivity, phase composition, particle size distribution and particle morphology. The prepared powders were applied to the organic matrix in mass tone, and their resulting colour hues shifted from copper brown via chocolate brown to dark brown. The NIR solar reflectance was calculated in the wavelength interval of 700–1650 nm following the ASTM 173-03 standard and their values of powder form were 25%–44%. The colour hue and NIR solar reflectance were dependent on the calcination temperature and the preparation method. The optimal condition for the preparation of the most NIR-reflective saturated brown pigment is the precipitation method and a temperature of 1050 °C (R_solar = 42%; C_{powder form} = 18.4), with an interesting matchstick shape of particles.     

Microstructure and mechanical properties of hot-pressed SiC nanofiber reinforced SiC composites

This study reports on the preparation and mechanical properties of a novel SiC_nf/SiC composite. The single crystal SiC nanofiber(SiC_nf) reinforced SiC ceramic matrix composites (CMC) were successfully fabricated by hot pressing the mixture of β-SiC powders, SiC_nf and Al–B–C powder. The effects of SiC_nf mass fraction as well as the hot-pressing temperature on the microstructure and mechanical properties of SiC_nf/SiC CMC were systematically investigated. The results demonstrated that the 15 wt% SiC_nf/SiC CMC obtained by hot pressing (HP) at 1850 °C with 30 MPa for 60 min possessed the maximum flexural strength and fracture toughness of 678.2 MPa and 8.33 MPa m^1/2, respectively. The nanofibers pull out, nanofibers bridging and cracks deflection were found by scanning electron microscopy, which are believed can strengthen and toughen the SiC_nf/SiC CMC via consuming plenty of the fracture energy. Besides, although the relative density of the prepared SiC_nf/SiC CMC further increased with the sintering temperature rose to 1900 °C, the further coarsend composites grains results in the deterioration of the mechanical properties for the obtained composites compared to 1850 °C.     

CO2 laser post-treatment of sol-gel-derived Y3Al5O12:Ce phosphor ceramic powders

Cerium-doped yttrium aluminum garnet (Y₃Al₅O₁₂:Ce, YAG:Ce) was prepared using a sol-gel method and then fired for CO₂ laser post-treatments. Phase transformations and formation of impurities were not observed in YAG:Ce after CO₂ laser sintering. The shift of the diffraction peak and the appearance of another Raman peak indicate a more homogeneous distribution of Ce activators and enhanced crystallinity in laser-sintered YAG hosts. Larger spheres (100–200 μm) with tiny crystallites (<10 μm) were observed on the smoother surface in the laser-sintered YAG:Ce, unlike the irregular, porous, and layered powders in the sol-gel-derived YAG:Ce (1–100 μm). Photoluminescence (PL) measurements revealed an emission increase of 180% and a red shift of the emission peak for the laser-sintered YAG:Ce powders compared with the sol-gel-derived powders. Both have comparable thermal PL quenching behavior; however, the YAG:Ce powders with CO₂ laser treatment exhibited a PL efficiency improvement of approximately 4%.     

SPS densification and microstructure of ZrB2 composites derived from sol–gel ZrC coating

A technique for densifying ultra high temperature ceramic composites while minimising grain growth is reported. As-purchased ZrB₂ powder was treated with a zirconia-carbon sol–gel coating. Carbothermal reduction at 1450 °C produced 100–200 nm crystalline ZrC particles attached on the surface of ZrB₂ powders. The densification behaviour of the sol–gel coated powder was compared with both the as-purchased ZrB₂ and a compositionally similar ZrB₂–ZrC mixture. All three samples were densified by spark plasma sintering (SPS). The ZrB₂ reference sample was slow to densify until 1800 °C and was not fully dense even at 2000 °C, while the sol–gel modified ZrB₂ powder completed densification by 1800 °C. The process was studied by ram displacement data, gas evolution, SEM, and XRD. The sol–gel coated nanoparticles on the ZrB₂ powder played a number of important roles in sintering, facilitating superior densification by carbothermal reduction, nanoparticle coalescence and solid-state diffusion, and controlling grain growth and pore removal by Zener pinning. The sol–gel surface modification is a promising technique to develop ultra-high temperature ceramic composites with high density and minimum grain growth.     

Synthesis and characterization of the crystalline powders on the basis of Lu2O3:Eu3+spherical submicron-sized particles

This study is devoted to the preparation of the crystalline powders on the basis of non-agglomerated monodisperse Lu₂O₃:Eu³⁺ spherical particles with the diameters in the range of 50–250 nm by the soft chemistry co-precipitation route. The influence of the synthesis parameters on control morphology, particles size and agglomeration in the final Lu₂O₃:Eu³⁺ powder was considered. Lu₂O₃:Eu³⁺ crystalline powders were characterized by means of electron microscopy methods (TEM, SEM), FT-IR spectroscopy, thermal analysis (TG-DTA) and X-ray diffractometry. The mechanisms of the precursor decomposition and crystallization at the temperatures ranging from 60 to 900 °C were discussed. It was shown that the powders obtained were characterized by the effective luminescence under X-ray excitation in λ = 575–725 nm spectral region corresponding to ⁵D₀ → ⁷F_J transitions (J = 0–4) of Eu³⁺ ions with a maximum at 612 nm and the luminescence intensity strongly depends on annealing temperature. The relative densities of the green-bodies on the basis of Lu₂O₃:Eu³⁺ powders were estimated and the sintering of compacts at the temperatures up to 1500 °C was studied.     

Bismuth titanates candidates for high permittivity LTCC

Bi₂O₃–TiO₂ composites are known to possess attractive microwave dielectric properties. However, producing LTCC analogues with equally promising dielectric properties is problematic. Here, we show that judicious choice of both TiO₂ starting powders and dopants can produce composites with excellent properties. Three TiO₂ powders were evaluated: 1 μm-anatase, 1 μm-rutile and a nanosized (30 nm) mixture of 75–25 anatase-rutile. The best dielectric properties were obtained by using uncalcined nanosized anatase/rutile with Bi₂O₃ powder. By doping this Bi₂O₃–TiO₂ powder mixture with 0.112 wt.% CuO dielectric properties of Q × f = 9000 GHz, ɛ_r = 80 and τ_f = 0 ppm/K (at 300 K) were obtained at a sintering temperature of 915 °C.     

Effects of starting powder on microstructure and thermal conductivity of pressureless-sintered fully ceramic microencapsulated fuels

The effects of the starting SiC powder (α or β) with the addition of 5.67 wt% AlN–Y₂O₃–CeO₂–MgO additives on the residual porosity and thermal conductivity of fully ceramic microencapsulated (FCM) fuels were investigated. FCM fuels containing ～41 vol% and ～37 vol% tristructural isotropic (TRISO) particles could be sintered at 1870 °C using α-SiC and β-SiC powders, respectively, via a pressureless sintering route. The residual porosities of the SiC matrices in the FCM fuels prepared using the α-SiC and β-SiC powders were 1.1% and 2.3%, respectively. The thermal conductivities of FCM pellets with ～41 vol% and ～37 vol% TRISO particles (prepared using the α-SiC and β-SiC powders, respectively) were 59 and 41 Wm^?1K^?1, respectively. The lower porosity and higher thermal conductivity of FCM fuels prepared using the α-SiC powder were attributed to the higher sinterability of the α-SiC powder than that of the β-SiC powder.     

Sinterability,microstructures and electrical properties of Ni/Sm-doped ceria cermet processed with nanometer-sized particles

Ni/Sm-doped ceria (SDC) cermet was prepared from two types of NiO/SDC mixed powders: Type A—Mechanical mixing of NiO and SDC powders of micrometer-sized porous secondary particles containing loosely packed nanometer-sized primary particles. The starting powders were synthesized by calcining the oxalate precursor formed by adding the mixed nitrate solution of Ce and Sm or Ni nitrate solution into oxalic acid solution. Type B—Infiltration of Ni(NO₃)₂ solution into the SDC porous secondary particles subsequently freeze-dried. Type B powder gave denser NiO/SDC secondary particles with higher specific surface area than Type A powder. The above two types powders were sintered in air at 1100–1300 °C and annealed in the H₂/Ar or H₂/H₂O atmosphere at 400–700 °C. Increased NiO content reduced the sinterability of Type A powder but the bulk density of Type B powder compact showed a maximum at 34 vol.% NiO (25 vol.% Ni). Type B cermet was superior to Type A cermet in achieving fine-grained microstructure and a homogeneous distribution of Ni and SDC grains. The electrical resistance of the produced cermet decreased drastically at 15 vol.% Ni for Type B and at 20 vol.% Ni for Type A.     

Alon-based materials prepared by SHS technique

The aim of the presented paper was preparation of the highly reactive in the sintering powders in the Al–O–N system by SHS method. Combustion reactions of metallic aluminium and corundum powder mixtures (from 15% Al–85% Al₂O₃ to 50% Al–50% Al₂O₃) were performed in nitrogen atmosphere. The obtained powders were ground and hot-pressed at 1750, 1850 and 1950 °C for 1 h under 25 MPa in nitrogen flow. In contrast to conventional methods, which require 24 h of the precursor heat treatment at 1200 °C our studies, showed that it is possible to prepare almost pure γ-alon materials using SHS reaction. Sintering of the powders led to obtained dense materials composed of pure γ-alon or γ-alon–AlN composites. The phase composition of the sintered bodies was controlled by the chemical composition of the starting mixture and the sintering temperature.     

Processing and properties of polycrystalline cubic boron nitride reinforced by SiC whiskers

Dense polycrystalline cBN (PcBN)–SiCw composites were fabricated by a two-step method: First, SiO₂ was coated on the surface of cubic boron nitride (cBN) particles by the sol-gel method. Then, silicon carbide whisker (SiC_w)- coated cBN powder was prepared by carbon thermal reaction between SiO₂ and carbon powders at 1500°C for 2 hour. Then, cBN–SiC_w complex powders were sintered by high-pressure and high-temperature sintering technology using Al, B, and C as sintering additives. The phase compositions and microstructures of cBN–SiC_w composites were investigated by X-ray diffraction and scanning electron microscopy, respectively. It was found that the SiC_w and Al₃BC₃ had been fabricated by in situ reaction, which cannot only promote densification but also improve mechanical properties. The relative density of PcBN composites increased from 96.3% to 99.4% with increasing SiC_w contents from 5 to 20 wt%. Meanwhile, the Vickers hardness, fracture toughness and flexural strength of as-obtained composites exhibited a similar trend as that of relative density. The composite contained 20 wt% of SiC_w exhibited the highest Vickers hardness and fracture toughness of 42.7 ± 1.9 GPa and 6.52 ± 0.21 MPa•m^1/2, respectively. At the same time, the flexural strength reached 406 ± 21 MPa.     

B4C–TiB2 composites fabricated by hot pressing TiC–B mixtures: The effect of B excess

Previous research have reported that B₄C–TiB₂ composites could be prepared by the reactive sintering of TiC–B powder mixtures. However, due to spontaneous oxidation of raw powders, using TiC–B powder mixtures with a B/TiC molar ratio of 6: 1 introduced an intermediate phase of C during the sintering process, which deteriorated the hardness of the composites. In this report, the effects of B excess on the phase composition, microstructure, and mechanical properties of B₄C–TiB₂ composites fabricated by reactive hot pressing TiC–B powder mixtures were investigated. XRD and Raman spectra confirmed that lattice expansion occurred in B-rich boron carbide and B_xC–TiB₂ (x > 4) composites were obtained. The increasing B content improved the hardness and fracture toughness but decreased the flexural strength of B_xC–TiB₂ (x > 4) composites. When the molar ratio of B/TiC increased from 6.6:1 to 7.8:1, the Vickers hardness and the fracture toughness of the composites were enhanced from 26.7 GPa and 4.53 MPa m^1/2 to 30.4 GPa and 5.78 MPa m^1/2, respectively. The improved hardness was attributed to the microstructural improvement, while the toughening mechanism was crack deflection, crack bridging and crack branching.     

Structure and mechanical properties of in-situ synthesized α-Ti/TiO2/TiC hybrid composites through mechanical milling and spark plasma sintering

The main aim of this study was to apply high-energy longer mechanical milling and spark plasma sintering (SPS) techniques to produce in-situ α-Ti/TiO₂/TiC hybrid composites from commercially pure-Ti (CP–Ti, HCP structure) powders. The CP-Ti powders were subjected to different milling times (0, 20, 40, 60, 80, 100, and 120 h). The results showed that the powder samples milled for 120 h produced Ti, Ti₃O₅, TiO, TiO₂ phases, and dissolved C atoms from the process control agent (toluene) which were then converted to α-Ti, TiO₂, and TiC phases (formed in-situ composites) through spark plasma sintering. This was expected due to more reactivity in the 120 h sample as longer milling introduces severe and robust structural refinements. Structural evaluations with increasing milling time were carried out using XRD, HRSEM, and HRTEM. The synthesized powders were then consolidated by SPS at pressures of 50 MPa and 1323 K for 6 min. The micro-hardness results have shown that the hardness was started to increase from 1.40 GPa to 5.56 GPa with increasing milling time due to more dislocation and pinning effect produced by grain refinement and formed TiO₂/TiC intermetallic particles enhancing the strength of α-Ti matrix. The α-Ti/TiO₂/TiC in-situ hybrid composite bulk sample yielded an ultimate compressive strength of 1.594 GPa.     

Alternating Current Electrophoretic Deposition of Antibacterial Bioactive Glass-Chitosan Composite Coatings

Alternating current (AC) electrophoretic deposition (EPD) was used to produce multifunctional composite coatings combining bioactive glass (BG) particles and chitosan. BG particles of two different sizes were used, i.e., 2 μm and 20–80 nm in average diameter. The parameter optimization and characterization of the coatings was conducted by visual inspection and by adhesion strength tests. The optimized coatings were investigated in terms of their hydroxyapatite (HA) forming ability in simulated body fluid (SBF) for up to 21 days. Fourier transform infrared (FTIR) spectroscopy results showed the successful HA formation on the coatings after 21 days. The first investigations were conducted on planar stainless steel sheets. In addition, scaffolds made from a TiAl4V6 alloy were considered to show the feasibility of coating of three dimensional structures by EPD. Because both BG and chitosan are antibacterial materials, the antibacterial properties of the as-produced coatings were investigated using E. coli bacteria cells. It was shown that the BG particle size has a strong influence on the antibacterial properties of the coatings.     

Fabrication and characterization of nanocrystalline Mg-substituted fluorapatite by high energy ball milling

The aim of this work was preparation and characterization of Mg-substituted nanostructured FA powders. Mg-substituted nanostructured FA powders were synthesized with a chemical composition of Ca_10?xMg_x(PO₄)₆F₂, with x=0, 0.5, 1, 1.5 and 2 by mechanical alloying method. Successful substitution of Ca²⁺ with Mg ions in the fluorapatite lattice was investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FTIR). The results showed that after 12 h of milling, pure nanocrystalline Mg-substituted FA powders with different Mg contents were synthesized. The incorporation of Mg ions into the fluorapatite caused the decrease of the lattice parameters. With increasing Mg content, the crystallinity of powder decreased while the degree of agglomeration of powder increased. SEM and TEM analysis showed that the powder was agglomerated and composed of nanocrystalline particles with the average particle size of less than 100 nm.