Preparation of 3D printed silicon nitride bioceramics by microwave sintering.

Silicon nitride (Si3N4) is a bioceramic material with potential applications. Customization and high reliability are the foundation for the widespread application of Si3N4 bioceramics. This study constructed a new microwave heating structure and successfully prepared 3D printed dense Si3N4 materials, overcoming the adverse effects of a large amount of 3D printed organic forming agents on degreasing and sintering processes, further improving the comprehensive performance of Si3N4 materials. Compared with control materials, the 3D printed Si3N4 materials by microwave sintering have the best mechanical performance: bending strength is 928 MPa, fracture toughness is 9.61 MPa·m1/2. Meanwhile, it has the best biocompatibility and antibacterial properties, and cells exhibit the best activity on the material surface. Research has shown that the excellent mechanical performance and biological activity of materials are mainly related to the high-quality degreasing, high cleanliness sintering environment, and high-quality liquid-phase sintering of materials in microwave environments.

Effect of AlN on the Mechanical and Electrochemical Properties of Aluminum Metal Matrix Composites.

In the present investigation, aluminum metal matrix composites (AMMs) reinforced with aluminum nitride (AlN) nanoparticulates at different volumetric ratios of (0, 0.5, 1, 1.5, and 2 vol.%) were manufactured via a microwave-assisted powder metallurgy technique. The morphological, physical, mechanical, and electrochemical properties of the produced billets were examined to reflect the impact of the successive addition of AlN into the aluminum (Al) matrix. The morphological analysis revealed the high crystalline patterns of the formation of the Al-AlN composites. The microstructural analysis confirmed the presence of the elemental constituents of Al and AlN particles in the fabricated composites, showing an enhanced degree of agglomeration in conjunction with the additional amount of AlN. Positive behavior exhibited by the micro- and nanohardness was noticeable in the Al-AlN composites, especially at the ultimate concentration of AlN in the Al matrix of a 2 vol.%, where it reached 669.4 ± 28.1 MPa and 659.1 ± 11 MPa compared to the pure Al metal at 441.2 ± 20 MPa and 437.5 ± 11 MPa, respectively. A declining trend in the compressive strength was recorded in the reinforced Al samples. The corrosion resistance of the AlN-reinforced Al metal matrix was estimated at 3.5 wt.% NaCl using electrochemical impedance spectroscopy and potentiodynamic polarization. The results reveal that the inclusion of 2.0 vol.%AlN led to the lowest corrosion rate.

Dental zirconia microwave-sintering followed by rapid cooling protocol.

OBJECTIVES: This study aimed to evaluate the effect of microwave sintering temperature and cooling rate (MS) on 3Y-TZP ceramics and its influence on the ceramic microstructure and mechanical properties. Specifically, to optimize the sintering process, reducing the total sintering time compared to conventional sintering. MATERIALS AND METHODS: Eighty-four pre-sintered Y-TZP discs (Vipi block Zirconn, VIPI) (ISO 6872) were divided into seven groups (n = 12) according to the sintering conditions: conventional sintering (CS) at 1530 °C for 120 min and microwave sintering at 1400 °C (MS1400) and 1450 °C (MS1450) for 15 min followed by different cooling conditions: rapid cooling (RC), cooling at 400 °C (C400) and 25 °C (C25). The specimens were submitted to apparent density measurements, X-ray diffraction analysis (XRD), scanning electron microscopy, and biaxial flexural strength test. Data was statistically analyzed through two-way ANOVA, Tukey, Sidak, Dunnett and Weibull (α = 0.05). RESULTS: All MS1400 groups presented lower density values than the CS and MS1450 groups. Two-way ANOVA revealed that the MS temperature and cooling rate affected the biaxial flexural strength of the Y-TZP (p < 0.01). Group MS1400RC presented lower biaxial flexural strength values (681.9 MPa) than MS1450RC (824.7 MPa). The cooling rate did not statistically decrease the biaxial strength among the groups submitted to microwave sintering at 1450 °C. XRD analysis showed that the sintering and cooling temperature did not induce tetragonal to monoclinic phase transformation. CONCLUSIONS: Microwave sintering at 1450 °C for 15 min followed by rapid cooling can be a viable fast alternative protocol for Y-TZP sintering, compared with the conventional sintering, reducing the total sintering time by 75% and reducing the energy used for the sintering process without affecting the Y-TZP biaxial flexural strength and relative density compared to the conventional sintering. Moreover, the microwave technique promoted smaller grains and did not induce monoclinic phase formation.

Silicon Nitride Bioceramics Sintered by Microwave Exhibit Excellent Mechanical Properties, Cytocompatibility In Vitro, and Anti-Bacterial Properties.

Silicon nitride is a bioceramic with great potential, and multiple studies have demonstrated its biocompatibility and antibacterial properties. In this study, silicon nitride was prepared by a microwave sintering technique that was different from common production methods. SEM and pore distribution analysis revealed the microstructure of microwave-sintered silicon nitride with obvious pores. Mechanical performance analysis shows that microwave sintering can improve the mechanical properties of silicon nitride. The CCK-8 method was used to demonstrate that microwave-sintered silicon nitride has no cytotoxicity and good cytocompatibility. From SEM and CLSM observations, it was observed that there was good adhesion and cross-linking of cells during microwave-sintered silicon nitride, and the morphology of the cytoskeleton was good. Microwave-sintered silicon nitride has been proven to be non-cytotoxic. In addition, the antibacterial ability of microwave-sintered silicon nitride against Staphylococcus aureus and Escherichia coli was tested, proving that it has a good antibacterial ability similar to the silicon nitride prepared by commonly used processes. Compared with silicon nitride prepared by gas pressure sintering technology, microwave-sintered silicon nitride has excellent performance in mechanical properties, cell compatibility, and antibacterial properties. This indicates its enormous potential as a substitute material for manufacturing bone implants.

Investigation of mechanical properties and low-temperature degradation of dental 3Y-TZP ceramics fabricated by stereolithography in combination with microwave sintering.

The purpose of this study was to obtain dental ceramic materials with excellent mechanical properties and high resistance to low temperature degradation (LTD) via stereolithography (SLA) in combination with microwave sintering (MWS). The results have shown that the unaged MWS-1425 °C 3Y-TZP ceramics with uniform microstructure have high density up to 99.04% and excellent mechanical properties (Vickers hardness 14.07 GPa, fracture toughness 4.32 MPa m1/2, flexural strength 947.87 MPa). After 50 h of LTD, the m-phase content of MWS 3Y-TZP ceramics accounts for only 10.3%. In addition, the surface roughness increases by only 1.3 nm, the degraded depth is less than 5 µm, and the flexural strength exceeds 900 MPa. This exhibits the high resistance to LTD and excellent mechanical properties of dental 3Y-TZP ceramics can be obtained.

The current status and future of solid waste recycled building bricks.

Solid waste (SW) has become a problem hindering the economic and social development. Achieving the full green cycle from raw material to production of recycled building bricks (RBB) using SW is the focus of future research. In this paper, the research results of RBB manufacturing using SW in recent years are reviewed. According to the consolidation principle of RBB, the effects of different types of SW on the physicochemical properties and microstructure of RBB are summarized based on the recycled unsintered brick (RUSB) and recycled sintered brick (RSB). By comparing and evaluating the two consolidation methods, it is proposed that RSB has good practicality due to its higher SW utilization rate, higher strength, and faster consolidation speed. Furthermore, the difference between MWS and conventional sintering (CS) is analyzed, and the research on the application of MWS in SW-RBB manufacturing in recent years is reviewed in detail. It is pointed out that microwave sintering (MWS) technology can solve many drawbacks in traditional sintering technology and has great prospects in manufacturing SW-RBB due to the low energy consumption, low pollution, and high efficiency. Finally, the shortcomings and possible challenges in the current research on manufacturing SW-RBB using MWS technology are discussed, which provides guidance for the future development of SW-RBB manufacturing.

Effects of irradiation behavior on physicochemical properties of glassy radioactive contaminated soil containing various contents of actinides nuclear waste.

The evaluation of radiation resistance of the treated radioactive contaminated soil is crucial. The irradiation behavior of simulated radioactive soil waste irradiated with 1.5 MeV Xe20+ ions at fluences of 1 × 1012-1 × 1015 ions/cm2 was studied. Before the irradiation experiment, all the samples were sintered by microwave. The results showed that microwave sintering may be used to treat radioactive contaminated soil. In addition, the irradiation experiment results show that when the Nd2O3 content was low (<20 wt.%), the irradiation has little effect on the sample. When the Nd2O3 content was higher, the Vickers hardness of the sample (25 wt.%) decreased by 7 % at a fluence of 1 × 1015 ions/cm2, which may be due to the high Nd2O3 content that destroyed the overall stability of the glass waste form. The low normalized leaching rate of the irradiated sample (LRNd, ∼10-6 g·m-2·d-1) also proved that it had good aqueous durability. Moreover, the radiation resistance of the sample was illustrated by studying the influence mechanism of 1.5 MeV Xe20+ irradiation on radioactive contaminated soil. This work can help to study the environmental pollution problems of radioactive contaminated soil containing various contents of actinide nuclear waste.

Resistive coupled microwave sintering of hydroxyapatite/titania nano-biocomposite and tailoring its mechanical properties.

Tailoring the mechanical properties of bioceramics plays a crucial role in the fabrication of hard tissue substitutes. In this work, phase pure nanostructured hydroxyapatite and titania were synthesized using a single-step combustion technique. To study the influence of titania in the mechanical properties of hydroxyapatite, hydroxyapatite/titania (TiO2-0%, 10%, 20%, and 30%) nanocomposites were prepared. The sample containing 20% titania showed maximum sinterability and was analysed in detail. The samples were sintered by a novel resistive coupled microwave sintering to 98.9% of the theoretical density at 1020 °C for a soaking duration of 20 min. A substantial reduction in sintering temperature of ∼165 °C and a significantly low soaking duration were observed in the samples sintered using the new technique and it yielded pellets with reduced grain size compared to the samples sintered via conventional resistive heating. They have shown better microhardness of 7.7 GPa, enhanced compressive strength of 194.9 MPa, and improved elastic modulus of 136.2 GPa without compromising the cell viability, cell adhesion, differentiation, proliferation, and biomineralization. The results indicate that by varying the titania content in hydroxyapatite and by adopting a suitable low-temperature sintering strategy like resistive coupled microwave sintering, one can tailor the mechanical properties of bone implants.

An Investigation into the Potential of Turning Induced Deformation Technique for Developing Porous Magnesium and Mg-SiO2 Nanocomposite.

A new and novel method of synthesising porous Mg materials has been explored utilising a variant of a processing method previously used for the synthesis of dense Mg materials, namely the turning-induced deformation (TID) method combined with sintering. It was found that the Mg materials synthesised possessed comparable properties to previously-synthesised porous Mg materials in the literature while subsequent sintering resulted in a more consistent mechanical response, with microwave sintering showing the most promise. The materials were also found to possess mechanical response within the range of the human cancellous bone, and when reinforced with biocompatible silica nanoparticles, presented the most optimal combination of mechanical properties for potential use as biodegradable implants due to most similarity with cancellous bone properties.

Characterization of AZ31/HA Biodegradable Metal Matrix Composites Manufactured by Rapid Microwave Sintering.

This study reports the development of magnesium alloy/hydroxyapatite-based biodegradable metal matrix composites (BMMCs) through rapid microwave sintering. Magnesium alloy (AZ31) and hydroxyapatite powder were used in four compositions 0, 10, 15 and 20% by weight. Developed BMMCs were characterized to evaluate physical, microstructural, mechanical and biodegradation characteristics. XRD results show Mg and HA as major phases and MgO as a minor phase. SEM results correlate with the XRD findings by identifying the presence of Mg, HA and MgO. The addition of HA powder particles reduced density and increased the microhardness of BMMCs. The compressive strength and Young's modulus increased with increasing HA up to 15 wt.%. AZ31-15HA exhibited the highest corrosion resistance and lowest relative weight loss in the immersion test for 24 h and weight gain after 72 and 168 h due to the deposition of Mg(OH)2 and Ca(OH)2 layers at the sample surface. XRD analysis of the AZ31-15HA sintered sample after an immersion test was carried out and these results revealed the presence of new phases Mg(OH)2 and Ca(OH)2 that could be the reason for enhancing the corrosion resistance. SEM elemental mapping result also confirmed the formation of Mg(OH)2 and Ca(OH)2 at the sample surface, which acted as protective layers and prevented the sample from further corrosion. It showed that the elements were uniformly distributed over the sample surface. In addition, these microwave-sintered BMMCs showed similar properties to the human cortical bone and help bone growth by depositing apatite layers at the surface of the sample. Furthermore, this apatite layer can enhance osteoblast formation due to the porous structure type, which was observed in the BMMCs. Therefore, it is indicative that developed BMMCs can be an artificial biodegradable composite for orthopedic applications.

Effect of Europium Addition on the Microstructure and Dielectric Properties of CCTO Ceramic Prepared Using Conventional and Microwave Sintering.

In this work, Eu2O3-doped (CaCu3Ti4O12)x of low dielectric loss have been fabricated using both conventional (CS) and microwave sintering (MWS), where x = Eu2O3 = 0.1, 0.2, and 0.3, respectively. According to X-ray diffraction (XRD) and scanning electron microscope (SEM) reports, increasing the concentration of Eu3+ in the CCTO lattice causes the grain size of the MWS samples to increase and vice versa for CS. The X-ray photoelectron spectroscopy (XPS) delineated the binding energies and charge states of the Cu2+/Cu+ and Ti4+/Ti3+ transition ions. Energy dispersive spectroscopy (EDS) analysis revealed no Cu-rich phase along the grain boundaries that directly impacts the dielectric properties. The dielectric characteristics, which include dielectric constant (ε) and the loss (tan δ), were examined using broadband dielectric spectrometer (BDS) from 10 to 107 Hz at ambient temperature. The dielectric constant was >104 and >102 for CS and MWS samples at x > 0.1, respectively, with the low loss being constant even at high frequencies due to the effective suppression of tan δ by Eu3+. This ceramic of low dielectric loss has potential for commercial applications at comparatively high frequencies.

Influence of Solid Loading on the Gel-Casting of Porous NiTi Alloys.

Porous NiTi alloys are widely applied in the field of medical implant materials due to their excellent properties. In this paper, porous NiTi alloys were prepared by non-aqueous gel-casting. The influence of solid loading on the process characteristics of slurries and the microstructure and mechanical properties of sintered samples were investigated. The viscosity and the stability of slurry significantly increased with the growth of solid loading, and the slurry had better process characteristics in the solid loading range of 40-52 vol.%. Meanwhile, the porosity and average pore diameter of the sintered NiTi alloys decreased with a rise in the solid loading, while the compressive strength increased. Porous NiTi alloys with porosities of 43.3-48.6%, average pore sizes of 53-145 µm, and compressive strengths of 87-167 MPa were fabricated by gel-casting. These properties meet the requirements of cortical bone. The results suggest that the pore structure and mechanical properties of porous NiTi products produced by gel-casting can be adjusted by controlling the solid loading.

Microstructure and Mechanical Properties of Porous NiTi Alloy Prepared by Integration of Gel-Casting and Microwave Sintering.

Porous NiTi alloys were manufactured by integration of gel-casting and microwave sintering. The effects of sintering temperature on porosity, compressive strength, pore morphology and phase composition of sintered samples were researched. The results show that the porosity and the mean pore diameter of porous NiTi alloys decrease with increasing sintering temperature, whereas the content of the NiTi phase, the elastic modulus and compressive strength of sintered samples increase. When the gel body with the solid loading of 50 vol.% is microwave sintered at 1000 °C for 30 min, porous NiTi alloys are obtained with the porosity of 38.9%, the compressive strength of 254 MPa, elastic modulus of 4 GPa, and predominant phase of NiTi. The results suggest that the method is suitable for rapid preparation of large-size and complex-shape personalized products similar to human bones at a low cost.

Physical, mechanical, and biological characterization of robocasted carbon nanotube reinforced microwave sintered calcium phosphate scaffolds for bone tissue engineering.

This study analyses the influence of the addition of Multi Walled Carbon Nanotubes (MWCNT) on the physical, mechanical, and biological behaviour of Calcium Phosphate (CP) bone scaffolds developed using the robocasting technique for bone regeneration. Three different mass percentages (0.5, 1, and 2 wt%) of MWCNT are added to the CP powder and a slurry is prepared using a CMC binder for printing the scaffolds. The scaffolds were printed in 2 infill ratios, 50 and 100%, and were sintered under an inert atmosphere in a microwave furnace which was then taken for various characterization studies. Physical characterisation studies revealed that the shrinkage rate of scaffolds is very low compared to other additive manufacturing techniques. The incorporation of 0.5 wt% of MWCNT produced the best results in mechanical characterization studies with a compressive strength of 10.38 MPa and 11.89 MPa for 50% and 100% infill ratios respectively. In Vitro Biocompatibility studies also proved that 0.5 wt% MWCNT samples are the most suitable for cell growth while the hemocompatibility tests showed that the samples are blood compatible. . The 100% infill samples fared better than the 50% samples in physical and mechanical properties. The results suggest that the MWCNT incorporated CP scaffolds can be used to treat critical size bone defects.

Resistive coupled microwave sintering - A promising technique to fabricate bioceramics with improved properties.

Enhancing the mechanical properties of biocompatible hydroxyapatite is one of the major challenges in the fabrication of bone implants. In this work, phase pure samples of nano-hydroxyapatite with an average crystallite size of 22 nm, were synthesized by a modified single-step combustion technique. The samples were sintered by a novel resistive coupled microwave sintering technique to 98.4% of theoretical density at 1030 °C for a soaking duration of 20 min. The new method yielded pellets with an average grain size of 0.12 ± 0.01 µm, that showed an improved Vickers microhardness of 7.1 GPa, enhanced young's modulus of 110.51 ± 1.8 GPa, and better compressive strength of 172 ± 10 MPa compared to those pellets sintered via conventional resistive heating. The sintered samples showed better cell viability, cell adhesion, proliferation, differentiation, and osteogenic potential. The enhanced mechanical properties achieved by resistive coupled microwave sintering without compromising the biological properties is a remarkable result that can effectively be used in the fabrication of high-quality bone substitutes.

Rapid solidification of simulated radioactive contaminated soil by continuous microwave sintering: Effects of temperature and doping level.

In order to find a rapid, efficient, safe and reliable treatment technology for radioactive contaminated soil, the microwave sintering method was used to sinter the simulated radioactive contaminated soil with different CeO2 content at 1100 °C, 1200 °C and 1300 °C for 30 min to achieve vitrification. The phase, microstructure, morphology, mechanical properties, and chemical durability of the sintered samples were investigated. XRD and SEM-EDS results showed that Ce4+ did not participate in the formation of the glass network, but was fixed in the glass network structure. The amorphous fraction of the samples sintered at 1300 °C can reach up to 98%. EDS results showed that the element distribution was uniform. In addition, the density and hardness values of the sintered matrices were in the range of 1.875-2.543 g/cm3 and 6.667-7.112 GPa, respectively. Our results show that the density and hardness values are related to the sintering temperature and CeO2 content. The normalized leaching rate of Ce in samples reached 10-7 g/(m2·d) after 28 d.

Osteogenesis Performance of Boronized Ti6Al4V/HA Composites Prepared by Microwave Sintering: In Vitro and In Vivo Studies.

The boronized Ti6Al4V/HA composite is deemed to be an important biomaterial because of its potential remarkable mechanical and biological properties. This paper reports the osteogenesis performance of the boronized Ti6Al4V/HA composite, which was prepared by microwave sintering of powders of Ti6Al4V, hydroxyapatite (HA), and TiB2 in high-purity Ar gas at 1050 °C for 30 min, as dental implant based on both cell experiments in vitro and animal experiments in vivo. The comparison between the boronized Ti6Al4V/HA composite and Ti, Ti6Al4V, and boronized Ti6Al4V in the terms of adhesion, proliferation, alkaline phosphate (ALP) activity, and mineralization of MG-63 cells on their surfaces confirmed that the composite exhibited the best inductive osteogenesis potential. It exerted a more significant effect on promoting the early osteogenic differentiation of osteoblasts and exhibited the maximum optical density (OD) value in the MTT assay and the highest levels of ALP activity and mineralization ability, primarily ascribed to its bioactive HA component, porous structure, and relatively rough micro-morphology. The in vivo study in rabbits based on the micro-computed tomography (micro-CT) analysis, histological and histomorphometric evaluation, and biomechanical testing further confirmed that the boronized Ti6Al4V/HA composite had the highest new bone formation potential and the best osseointegration property after implantation for up to 12 weeks, mainly revealed by the measured values of bone volume fraction, bone implant contact, and maximum push-out force which, for example, reached 48.64%, 61%, and 150.3 ± 6.07 N at the 12th week. Owing to these inspiring features, it can serve as a highly promising dental implant.

Characteristics of Conventional and Microwave Sintered Iron Ore Preform.

In this study, compacted hematite (Fe2O3) preforms were made and sintered at various temperatures, such as 1250 °C and 1300 °C, using both conventional and microwave sintering methods. The density, porosity, microhardness, cold crushing strength, microphotographs, and X-ray diffraction (XRD) analysis of the sintered preforms were used to evaluate the performance of the two sintering methods. It was found that microwave sintered preforms possessed lesser porosity and higher density than conventionally sintered preforms owing to uniform heating of the powdered ore in microwave sintering method. Furthermore, it was also observed that microwave sintered preforms exhibited relatively higher cold crushing strength and hardness than conventionally sintered preforms. Thus, the overall results revealed that microwave sintering yielded better properties considered in the present study.

Ag metal interconnect wires formed by pseudoplastic nanoparticles fluid imprinting lithography with microwave assistant sintering.

Nanoimprint technology has the advantages of low cost, high precision, high fidelity and high yield. The metal nanoparticle fluid is non-Newtonian fluid, which is used as the imprint transfer medium to realize high fidelity of pattern because of its shear thinning effect. In order to functionalize the metal nanoparticles microstructure, the subsequent sintering step is required to form a metal interconnect wire. Metal interconnect wire with fewer grain boundaries and fewer holes have excellent mechanical and electronic properties. In this paper, the pseudoplastic metal nanoparticle fluid was formed by Ag nanoparticle and precursor solution, and then the thermal diffusion process was completed by microwave sintering after interconnects were embossed. The influence of microwave and thermal atmosphere on the microstructure and performance of Ag Interconnect wires was analyzed and discussed, and the Ag Interconnect wires performance was determined under the influence of time and temperature parameters. In our experiments, the interconnects after microwave sintering can achieve 39% of the conductivity of bulk silver. The microwave sintering module might be integrated as the heat treatment module of the metal micro/nano pattern directly imprint lithography.

Realization of Phase and Microstructure Control in Fe/Fe2SiO4-FeAl2O4 Metal-Ceramic by Alternative Microwave Susceptors.

This study provides a novel method to prepare metal-ceramic composites from magnetically selected iron ore using microwave heating. By introducing three different microwave susceptors (activated carbon, SiC, and a mixture of activated carbon and SiC) during the microwave process, effective control of the ratio of metallic and ceramic phases was achieved easily. The effects of the three susceptors on the microstructure of the metal-ceramics and the related reaction mechanisms were also investigated in detail. The results show that the metal phase (Fe) and ceramic phase (Fe2SiO4, FeAl2O4) can be maintained, but the metal phase to ceramic phase changed significantly. In particular, the microstructures appeared as well-distributed nanosheet structures with diameters of ~400 nm and thicknesses of ~20 nm when SiC was used as the microwave susceptor.