Resorbable, porous glass scaffolds by a salt sintering process

Resorbable, porous glass scaffolds for tissue engineering were prepared by sintering borate glass with salt (sodium chloride). Subsequently, the sodium chloride was dissolved in water resulting in a highly porous material. By modifying the process parameters including salt particle size, salt volume percentage, sintering temperature and sintering time, sintered matrix structures were optimized. Analysis of the structure data indicates that the 50 vol% glass—50 vol% salt with particle sizes from 250–315 μm sintered at a temperature of 520°C for 10 min resulted in an optimum structure with 76.5% porosity and 29.3 N/cm² compressive strength. The process of HAP formation on the scaffolds in 0.25 M K₂HPO₄ solutions with pH 9.0 at 37°C was evaluated. The structural changes were analyzed by X-ray diffraction and scanning electron microscopy. An amorphous phosphate was formed on the surface of the scaffolds within 1d and crystalline hydroxyapatite (HA) within 10d.     

The effect of processing parameters and solid concentration on the mechanical and microstructural properties of freeze-casted macroporous hydroxyapatite scaffolds

The design and fabrication of macroporous hydroxyapatite scaffolds, which could overcome current bone tissue engineering limitations, have been considered in recent years. In the current study, controlled unidirectional freeze-casting at different cooling rates was investigated. In the first step, different slurries with initial hydroxyapatite concentrations of 7–37.5 vol.% were prepared. In the next step, different cooling rates from 2 to 14 °C/min were applied to synthesize the porous scaffold. Additionally, a sintering temperature of 1350 °C was chosen as an optimum temperature. Finally, the phase composition (by XRD), microstructure (by SEM), mechanical characteristics, and the porosity of sintered samples were assessed. The porosity of the sintered samples was in a range of 45–87% and the compressive strengths varied from 0.4 MPa to 60 MPa. The mechanical strength of the scaffolds increased as a function of initial concentration, cooling rate, and sintering temperature. With regards to mechanical strength and pore size, the samples with the initial concentration and the cooling rate of 15 vol.% and 5 °C/min, respectively, showed better results.     

Effect of sintering temperature and cooling rate on the morphology, mechanical behavior and apatite-forming ability of a novel nanostructured magnesium calcium silicate scaffold prepared by a freeze casting method

In this research, sol–gel-derived nanostructured calcium magnesium silicate (merwinite)-based scaffolds were fabricated by water-based freeze casting method. The effect of cooling rate and sintering temperature on pore sizes and mechanical characteristics of the scaffolds was studied. Microstructure and surface morphology of scaffolds were also observed by scanning electron microscopy before and after various time intervals of soaking in simulated body fluid. The results showed that increasing temperature at the constant rate led to increasing the parameters of volume and linear shrinkage, strength (σ), and Young’s modulus (E) but decreasing porosity. This increase was significant for strength and Young’s modulus. In addition, with the increase of rate at the constant temperature, the parameters of volume and linear shrinkage and also porosity decreased whereas strength and Young’s modulus increased significantly. According to the obtained mechanical results, the best mechanical properties were achieved when the scaffold was prepared at cooling rate and sintering temperature of 277.15°K/min and 1623.15°K, respectively (E = 0.048 GPa and σ = 2 MPa). These values were closer to the lower limit of the values for cancellous bone. The acellular in vitro bioactivity revealed that different apatite morphologies were formed on the surfaces for various periods of soaking time when the scaffolds prepared at the freezing temperature of 277.15°K/min and at the two different sintering temperatures. The favorable mechanical behavior of the porous constructs, coupled with the ability of forming apatite particles on the surface of scaffold, indicates the potential of the present freeze casting route for the production of porous scaffolds for bone tissue engineering.     

3D printed porous β-Ca2SiO4 scaffolds derived from preceramic resin and their physicochemical and biological properties

Silicate bioceramic scaffolds are of great interest in bone tissue engineering, but the fabrication of silicate bioceramic scaffolds with complex geometries is still challenging. In this study, three-dimensional (3D) porous β-Ca₂SiO₄ scaffolds have been successfully fabricated from preceramic resin loaded with CaCO₃ active filler by 3D printing. The fabricated β-Ca₂SiO₄ scaffolds had uniform interconnected macropores (ca. 400 μm), high porosity (>78%), enhanced mechanical strength (ca. 5.2 MPa), and excellent apatite mineralization ability. Importantly, the results showed that the increase of sintering temperature significantly enhanced the compressive strength and the scaffolds sintered at higher sintering temperature stimulated the adhesion, proliferation, alkaline phosphatase activity, and osteogenic-related gene expression of rat bone mesenchymal stem cells. Therefore, the 3D printed β-Ca₂SiO₄ scaffolds derived from preceramic resin and CaCO₃ active fillers would be promising candidates for bone tissue engineering.     

Preparation of high strength macroporous hydroxyapatite scaffold

Hydroxyapatite (HAp) powder was prepared from CaNO₃·4H₂O and (NH₄)₂HPO₄ by wet-chemical method and has phase stable up to 1250 °C. High strength macroporous HAp–naphthalene (HN) and HAp–naphthalene–benzene (HNB) scaffolds were fabricated by adapting sintering method. The resulting HAp scaffolds have porosity about 60 vol.% with compressive strength of ~ 11 MPa and average pore diameter in the range of ~ 125 μm. The incorporation of benzene in HN scaffold reduces the strength whereas enhanced both the porosity and pore size distribution. XRD, FTIR, SEM and mercury porosimeter techniques were used to study the phase purity, morphology, pore size and pore size distribution of scaffold. The study compared the effect of concentration of naphthalene on strength, porosity and pore size distribution on both HN and HNB scaffold. In-vitro bioactivity studies on HN and HNB scaffolds show the nucleation of spherical carbonated apatite particles on the surface in SBF solution.     

Mechanical properties of hydroxyapatite–zirconia compacts sintered by two different sintering methods

Microwave sintering is traditionally employed to reduce the sintering temperature required to densify powder compacts. The effect of microwave heating on hydroxyapatite (HA)–zirconia (ZrO₂) green bodies has been investigated in order to understand how microwave energy may affect the physical and mechanical properties of the resultant densified composites. Laboratory synthesised nano-sized HA and a commercial nano-sized ZrO₂ powder have been ball milled to create mixtures containing 0–5 wt% ZrO₂ loadings. Compacts were microwave sintered at either 700, 1000 or 1200°C with a 1 h hold time. Comparative firings were also performed in a resistive element furnace using the same heating profile in order to assess the differences between conventional and microwave heating on the physical, mechanical and microstructural properties of the composites. Samples sintered at 700°C show little sign of densification with open porosities of approximately 50%. Composites conventionally sintered at 1000°C were between 65 and 75% dense, whereas the samples microwave sintered at this temperature were between 55 and 65% dense. Samples sintered at 1200°C showed the greatest degree of densification (>80%) with a corresponding reduction in open porosities. TCP generation occurred as a consequence of sintering at 1200°C, even with 0 wt% ZrO₂, and increased degradation of the HA phase to form significant amounts of TCP occurred with increasing additions of ZrO₂, along with increasing open porosity. Nanosized ZrO₂ prevents the densification of the HA matrix by effectively pinning grain boundaries and this effect is more pronounced in the MS materials. Similar strengths are achieved between the microwave and conventionally sintered samples. Greater amount of open porosity and pore interconnectivity are seen in the MS samples, which are considered to be useful for biomedical applications as they can promote osteo-integration.     

Vital role of hydroxyapatite particle shape in regulating the porosity and mechanical properties of the sintered scaffolds

The effect of particle shape on the porosity and compressive strength of porous hydroxyapatite (HA) scaffolds was investigated by sintering the mixture of rod-shaped HA (r-HA) and spherical HA (s-HA) with polyacrylamide used as the sacrificial template. It was found, for the first time, that addition of r-HA into s-HA could exponentially decrease the porosity of sintered HA scaffolds and enhance their compressive strength with the increase of r-HA content. The mechanism, according to the results from scanning electron microscopy and X-ray diffraction, lies in the restriction of s-HA to the grain formation and growth of r-HA during sintering and results in the fusion of r-HA with s-HA. These findings suggest that mixture of r-HA and s-HA might provide a new and facile way to improve the compressive strength of porous HA scaffolds.     

Magnetic,optical, dielectric,and sintering properties of nano-crystalline BaFe<Subscript>0.5</Subscript>Nb<Subscript>0.5</Subscript>O<Subscript>3</Subscript> synthesized by a polymerization method

A one-pot polymerization method using citric acid and glucose for the synthesis of nano-crystalline BaFe_0.5Nb_0.5O₃ is described. Phase evolution and the development of the crystallite size during decomposition of the (Ba,Fe,Nb)-gel were examined up to 1100 °C. Calcination at 850 °C of the gel leads to a phase-pure nano-crystalline BaFe_0.5Nb_0.5O₃ powder with a crystallite size of 28 nm. The shrinkage of compacted powders starts at 900 °C. Dense ceramic bodies (relative density ≥ 90%) can be obtained either after conventional sintering above 1250 °C for 1 h or after two-step sintering at 1200 °C. Depending on the sintering regime, the ceramics have average grain sizes between 0.3 and 52 µm. The optical band gap of the nano-sized powder is 2.75(4) eV and decreases to 2.59(2) eV after sintering. Magnetic measurements of ceramics reveal a Néel temperature of about 23 K. A weak spontaneous magnetization might be due to the presence of a secondary phase not detectable by XRD. Dielectric measurements show that the permittivity values increase with decreasing frequency and rising temperature. The highest permittivity values of 10.6 × 10⁴ (RT, 1 kHz) were reached after sintering at 1350 °C for 1 h. Tan δ values of all samples show a maximum at 1–2 MHz at RT. The frequency dependence of the impedance can be well described using a single RC-circuit.     

Formation of water-soluble and biocompatible TOPO-capped CdSe quantum dots with efficient photoluminescence

Hollow hydroxyapatite (HA) microspheres (diameter = 100–800 μm) were prepared by reacting solid Li₂O–CaO–B₂O₃ glass spheres in 0.25 M K₂HPO₄ solution at 37°C. The influence of subsequent heating on the microstructure, surface area, and compressive strength of the HA microspheres was evaluated using scanning electron microscopy, the BET method, and nano-mechanical testing. The surface area and rupture strength of the as-prepared microspheres were 135 m²/g and 1.6 ± 0.6 MPa, respectively. On heating for 8 h at 600°C, the surface area decreased to 27 m²/g, but there was no increase in the compressive strength (1.7 ± 0.4 MPa). Heating to 800°C (8 h) resulted in a marked decrease in the surface area (to 2.6 m²/g) and a sharp increase in the compressive strength (to >35 ± 8 MPa). These hollow HA microspheres may be useful as devices for drug or protein growth factor delivery or as scaffolds for engineered tissues.     

Properties of porous Si3N4 ceramic electromagnetic wave transparent materials prepared by technique combining freeze drying and oxidation sintering

A simple and low-cost technique combining freeze drying and oxidation sintering is explored to prepare Si₃N₄ ceramics with high porosity and complex shape. The effects of sintering temperature and time on the phase composition, microstructure, porosity, pore size and dielectric constant of the porous Si₃N₄ ceramics are studied. Due to the variations of phase composition and microstructure, the porous Si₃N₄ ceramics sintered at different temperature possess characteristic in flexural strength. The porous Si₃N₄ ceramics sintered at 1,300 °C for 2–3 h have the highest flexural strength of 71–74 MPa. The changes of porosity and composition have much effect on the dielectric constant of porous Si₃N₄ ceramics. Because of the high porosity and SiO₂ volume fraction, the porous Si₃N₄ ceramics sintered at 1,300 °C for 2–3 h possess low dielectric constant of 3.4–3.6 and small pore size of 0.9 μm. The porous Si₃N₄ ceramics are good structural/functional and promising electromagnetic wave transparent material.     

Biomorphous porous hydroxyapatite-ceramics from rattan (<Emphasis Type="Italic">Calamus Rotang</Emphasis>)

The three-dimensional, highly oriented pore channel anatomy of native rattan (Calamus rotang) was used as a template to fabricate biomorphous hydroxyapatite (Ca₅(PO₄)₃OH) ceramics designed for bone regeneration scaffolds. A low viscous hydroxyapatite-sol was prepared from triethyl phosphite and calcium nitrate tetrahydrate and repeatedly vacuum infiltrated into the native template. The template was subsequently pyrolysed at 800°C to form a biocarbon replica of the native tissue. Heat treatment at 1,300°C in air atmosphere caused oxidation of the carbon skeleton and sintering of the hydroxyapatite. SEM analysis confirmed detailed replication of rattan anatomy. Porosity of the samples measured by mercury porosimetry showed a multimodal pore size distribution in the range of 300 nm to 300 μm. Phase composition was determined by XRD and FT-IR revealing hydroxyapatite as the dominant phase with minimum fractions of CaO and Ca₃(PO₄)₂. The biomorphous scaffolds with a total porosity of 70–80% obtained a compressive strength of 3–5 MPa in axial direction and 1–2 MPa in radial direction of the pore channel orientation. Bending strength was determined in a coaxial double ring test resulting in a maximum bending strength of ~2 MPa.     

Preparation and characterization of a novel willemite bioceramic

Willemite (Zn₂SiO₄) ceramics were prepared by sintering the willemite green compacts. The effects of sintering temperature on the linear shrinkage, porosity and mechanical strength of the ceramics were examined. With the sintering temperature increased, the linear shrinkage of the ceramics increased and the porosity decreased. When sintered at 1,300°C, willemite ceramics showed mechanical properties of the same order of magnitude as values for human cortical bone, as measured by bending strength (91.2 ± 4.2 MPa) and Young’s modulus (37.5 ± 1.5 GPa). In addition, the adhesion and proliferation of rabbit bone marrow stromal cells (BMSCs) on willemite ceramics was investigated. The results showed that the ceramics supported cell adhesion and stimulated the proliferation. All these findings suggest that willemite ceramics possess suitable mechanical properties and favorable biocompatibility and might be a promising biomaterial for bone implant applications.     

Effect of sintering temperature on the dielectric and varistor properties of SnO<Subscript>2</Subscript>–Zn<Subscript>2</Subscript>SnO<Subscript>4</Subscript> composite ceramics

The effect of sintering temperature from 1350 to 1450 °C on the dielectric and varistor properties of SnO₂–Zn₂SnO₄ composite ceramics has been systematically investigated. With the increasing of sintering temperature, the average grain size increased from about 1 to 5 μm and the breakdown electric field decreased from 117 to 3 V/mm. The relative dielectric constant increased with sintering temperature and it achieved the maximum of 1.2 × 10⁴ (40 Hz, 0 °C) at 1425 °C. With excessive increasing of sintering temperature, the relative dielectric constant decreased and the microstructure of the ceramic bulk became porous. In the spectra of imaginary part of the complex modulus, a peak was exhibited and the peak’s position shifted to high frequency with increasing testing or sintering temperature. The activation energy related to the peak was about 0.4 eV and this value was thought to be associated with the oxygen vacancies. Based on the sintering effect, the mechanism of oxygen vacancies in SnO₂–Zn₂SnO₄ composite ceramics was proposed and accordingly, the varistor and giant permittivity properties are well understood based on the grain boundary barrier model.     

Sintering behaviour and mechanical properties of Cr3C2–NiCr cermets

Cr₃C₂–NiCr cermets are used as metal cutting tools due to their relatively high hardness and low sintering temperatures. In this study, a powder mixture consisting of 75 wt% Cr₃C₂–25 wt% NiCr was sintered at four different temperatures and characterized for its microstructure and mechanical properties. The highest relative density obtained was 97% when sintered at 1350 °C. As the relative density increased, elastic modulus, transverse rupture strength, fracture toughness and hardness of the samples reached to a maximum of 314 GPa, 810 MPa, 10·4 MPa·m^1/2 and 11·3 GPa, respectively. However, sintering at 1400 °C caused further grain growth and pore coalescence which resulted in decreasing density and degradation of all mechanical properties. Fracture surface investigation showed that the main failure mechanism was the intergranular fracture of ceramic phase accompanied by the ductile fracture of the metal phase which deformed plastically during crack propagation and enhanced the fracture toughness.     

Synthesis of Iron-Based Friction Material by in Situ Reactive Sintering from Vanadium-Bearing Titanomagnetite

Based on the thermodynamic analyses, an iron-based friction material has been prepared directly from the vanadium-bearing titanomagnetite concentrates by means of a prereduction process and a final sintering process. Thermodynamically, ferrous oxides, titanium oxides, and vanadium oxides in the vanadium-bearing titanomagnetite concentrates can be converted to metal iron, titanium carbide, and vanadium carbide, respectively, by carbon at 1300°C in a vacuum of 10 Pa. During the process of prereduction, the percentage of ferrous oxides reduced to metal iron is about 96%, the percentage of FeTiO₃ converted into TiC is about 75%, and the percentage of V₂O₅ converted into VC is about 94%. During the process of final sintering, the samples were sintered at 1000°C for 3 h. The density, compressive strength, and Brinell hardness of this iron-based friction material are 5.07 g · cm^?3, 154.82 MPa, and 64 HBW, respectively. Its porosity ratio is about 18%. The stable coefficient of friction between this iron-based friction material and GCr15 is about 0.57 and the corresponding wear rate is 1.0145 × 10^?7 cm³ · J^?1. Consequently, the two-stage process presented in this paper can not only utilize the vanadium-bearing titanomagnetite concentrates effectively, but also find an alternative method to produce iron-based friction material economically.     

Effects of sintering processes on the element chemical states of In,Sn and O in ITO targets

The element chemical states of In, Sn and O could affect the resistivity of ITO targets so as to affect the electrical property of ITO films. In the work, nine kinds of ITO targets were prepared in order to investigate the effects of sintering processes on the element chemical states of In, Sn and O in ITO targets by XPS. The results show that the heating rate of 60 °C/h, the sintering temperature of 1580 °C, the holding time of 5 h and the cooling rate of 240 °C/h are favorable for the preparation of ITO targets with the optimum conductivity. The change rule of the element chemical states of In, Sn and O in ITO targets sintered with different sintering process parameters has been proved by the theoretical analysis of thermal decomposition kinetics of In₂O₃ and SnO₂.     

Application of metal injection molding process to fabrication of bulk parts of TiAl intermetallics

In the present study, a metal injection molding (MIM) process was applied to the fabrication of bulk parts of TiAl intermetallics, and effects of sintering parameters on densification of fabricated parts were investigated. The specimens sintered at 1350 °C showed about the same densification as the ones sintered at 1400 °C, while grains and pores were finer, and thus 1350 °C was chosen as the sintering temperature. In the sintered specimens after debinded in an H₂ atmosphere, Al₂O₃ precipitates were observed around pores. The densification decreased with increasing heating rate up to the sintering temperature. It was also found that the sintering time increased the densification without grain coarsening. The optimal heating rate was found to be 3 °C/min, and the densification reached a near-full level of 98.8% when sintered at 1350 °C for 30 h. These findings suggested a useful idea to successfully fabricate TiAl intermetallic parts by the MIM process.     

Effects of MnO2 and sintering temperature on microstructure, ferroelectric, and piezoelectric properties of Ba0.85Ca0.15Ti0.90Zr0.10O3 lead-free ceramics

Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ + xmol% MnO₂ lead-free ceramics have been prepared by a conventional sintering method and the effects of MnO₂ and sintering temperature on microstructure, ferroelectric, and piezoelectric properties of Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ lead-free ceramics have been studied. The addition of 0.25 mol% MnO₂ promotes grain growth, improves the ferroelectricity of the ceramics and strengthens ferroelectric tetragonal–ferroelectric orthorhombic phase transition near 40 °C. Because of the coexistence of tetragonal and orthorhombic phases and the combinatory effects of soft and hard doping of Mn ions, the ceramic with x = 0.25 exhibits the optimum piezoelectric properties (d ₃₃ = 306 pC/N and k _p = 42.2 %, respectively). Excess MnO₂ inhibits the grain growth and degrades the ferroelectric and piezoelectric properties of the ceramics. Sintering temperature has an important influence on the microstructure, tetragonal–orthorhombic phase transition near 40 °C, ferroelectric and piezoelectric properties of the ceramics. The increase in sintering temperature leads to large grains and more noticeable tetragonal–orthorhombic phase transition near 40 °C, enhances ferroelectricity and thus improves effectively the piezoelectricity of the ceramics. The Ba_0.85Ca_0.15Ti_0.90Zr_0.10O₃ ceramic sintered at 1350 °C possesses the optimum piezoelectric constant d ₃₃ value of 373 pC/N.     

Investigation the glazability of dimension andesites with glaze coating materials containing boron minerals in construction sector

This study examined the usability of thin plates cut from rocks of volcanic origin as new decorative indoor and outdoor coating material when used instead of ceramic saddle. The study examined the basic material characterization of andesites and the glazability of andesites with glaze coating materials containing boron minerals. The series of characterization tests were conducted on andesite samples. Then, the samples were applied glaze for trial purposes. Analysis indicated that the andesite samples consisted of sanidine, mica and pyroxene minerals and its apparent porosity, density, water absorption, salt crystallization resistance, compressive strength, frost after compressive strength, bending strength and impact resistance values were 15.75 %, 2,640 kg/m³, 7.41 %, 1.06 %, 47.03 MPa, 45.25 MPa, 10.16 MPa and 9.87 kPa respectively. In heat microscope measurements, maximum sintering was recorded at 1,182 °C. Linear expansion coefficient (α) of the andesite at 400 °C was 4.69 × 10^?6 K^?1. Firing performed by using the prepared glaze recipe at approximately 1,055 and 1,000 °C produced good results in terms of body-glaze harmony.     

Preparation and characterization of NiMn2O4 negative temperature coefficient ceramics by solid-state coordination reaction

The influence of synthesis parameters, such as calcination temperature and sintering temperature, on the microstructure, phase composition, and electrical properties of NiMn₂O₄ negative temperature coefficient (NTC) ceramics was systematically investigated. The NiMn₂O₄ NTC ceramics were synthesized via solid-state coordination reaction. With increasing sintering temperatures, the relative density increased, whereas the porosity decreased. Single-phase, cubic spinel ceramic was obtained following sintering at 900 and 1,050 °C, whereas a secondary phase, i.e., NiO, was detected when the sintering temperature was higher than 1,100 °C. High-density ceramics were obtained when the sintering temperature was higher than 1,100 °C, and featured the lowest room temperature resistivity of 2,924 Ω cm and thermal constant B of 3,429 K. The latter parameter reflects the temperature sensitivity of the NTC ceramics. Variations of the electrical property were because of increases in density and onset of decomposition.