Low-temperature hot-press sintering of AlN ceramics with MgO–CaO–Al2O3–SiO2 glass additives for ceramic heater applications

Aluminum nitride (AlN) is used a ceramic heater material for the semiconductor industry. Because extremely high temperatures are required to achieve dense AlN components, sintering aids such as Y₂O₃ are typically added to reduce the sintering temperature and time. To further reduce the sintering temperature, in this study, a low-melting-temperature glass (MgO–CaO–Al₂O₃–SiO₂; MCAS) was used as a sintering additive for AlN. With MCAS addition, fully dense AlN was obtained by hot-press sintering at 1500 °C for 3 h at 30 MPa. The mechanical properties, thermal conductivity, and volume resistance of the sintered AlN–MCAS sample were evaluated and compared with those of a reference sample (AlN prepared with 5 wt% Y2O3 sintering aid sintered at 1750 °C for 8 h at 10 MPa). The thermal conductivity of AlN prepared with 0.5 wt% MCAS was 91.2 W/m?K, which was 84.8 W/m?K lower than that of the reference sample at 25 °C; however, the difference in thermal conductivity between the samples was only 14.2 W/m?K at the ceramic-heater operating temperature of 500 °C. The flexural strength of AlN–MCAS was 550 MPa, which was higher than that of the reference sample (425 MPa); this was attributed to the smaller grain size achieved by low-temperature sintering. The volume resistance of AlN–MCAS was lower than that of the reference sample in the range of 200–400 °C. However, the resistivity of the proposed AlN–MCAS sample was higher than that of the reference sample (500 °C) owing to grain-boundary scattering of phonons. In summary, the proposed sintering strategy produces AlN materials for heater applications with low production cost, while achieving the properties required by the semiconductor industry.     

Comparative study of microwave absorption properties of Ni–Zn ferrites obtained from different synthesis technologies

Spinel ferrites are widely used for electromagnetic wave (EMW) absorption applications. In this study, spinel Ni–Zn ferrites with excellent microwave absorption properties were synthesized. Their EMW absorption characteristics and interaction mechanisms were studied to lay the foundation for the study of the role of Ni–Zn ferrite as a magnetic substrate for composites. Herein, Ni_0·5Zn_0·5Fe₂O₄ was prepared by the hydrothermal method (H-NZFO) and the sol–gel auto-combustion method (S-NZFO); both samples exhibited distinct microwave absorption properties. The S-NZFO absorber (thickness = 3.72 mm) demonstrated the best dual-zone microwave absorption with two strong reflection loss peaks at 5.1 and 10.5 GHz. The corresponding effective absorption bandwidth (EAB) reached 9.0 GHz, which covered part of the S-band and all of the C- and X-bands. These results were attributed to the high saturation magnetization, outstanding complex permeability, and multiple magnetic loss channels of S-NZFO. The H-NZFO sample exhibited excellent absorption capability and matching thickness. At a thickness as low as 1.71 mm, the minimum reflection loss (RL_min) of the H-NZFO absorber reached -60.2 dB at 13.1 GHz. The maximum bandwidth corresponding to RL below -10 dB was 4.6 GHz. These results can be attributed to small particle size, high complex permittivity, and multiple dielectric loss channels of H-NZFO. The observed wide effective absorption bandwidth of S-NZFO and strong microwave absorption capability of H-NZFO suggest the potential of both materials as substrates for efficient microwave absorbers in military as well as civilian absorption applications.     

Ultra-high temperature ceramics based on ZrB2 obtained by pressureless sintering with addition of Cr3C2, Mo2C,and WC

ZrB₂-MeC and ZrB₂-19 vol% SiC-Me_xC_y where Me=Cr, Mo, W were obtained by pressureless sintering. The capability to promote densification of ZrB₂ and ZrB₂-SiC matrices is the highest for WC and lowest for Cr₃C₂. The interaction between the components results in the formation of new phases, such as MeB (MoB, CrB, WB), a solid solution based on ZrC, and a solid solution based on ZrB₂. The addition of Cr₃C₂ decreases the mechanical properties. On the other hand, the addition of Mo₂C or WC to ZrB₂-19 vol% SiC composite ceramics leads increased mechanical properties. Long-term oxidation of ceramics at 1500 °C for 50 h showed that, in binary ZrB₂-Me_xC_y, a protective oxide scale does not form on the surface thus leading to the destruction of the composite. On the contrary, triple composites showed high oxidation resistance, due to the formation of dense oxide scale on the surface, with ZrB₂-SiC-Mo₂C displaying the best performance.     

Simultaneously enhancing mechanical and microwave absorption properties of Cf/SiC composites via SiC nanowires additions

C_f/SiC composite is an excellent structural and functional material, silicon carbide nanowires (SiCnws) are not only a toughening material but also a great application in the field of microwave absorption. In this study, SiCnws are grown on the surface of carbon fiber (C_f) by polymer impregnation and pyrolysis, and the SiC matrix was prepared by chemical vapor osmosis method. The SiCnws are introduced to enhance the mechanical and microwave absorption properties simultaneously. After 3 impregnations, the flexural strength of the composite was 107.35 ± 10 MPa. When the thickness is 1.86 mm, the minimum reflection loss value is ?41.08 dB, and the effective absorption bandwidth (RL ≤ ?10 dB) is 3.86 GHz. Furthermore, the microwave absorption mechanism of the material is discussed. This work provides a new method to prepare lightweight, stable and high-performance microwave absorption materials, and these materials are expected to be used in high temperature environments.     

Dielectric and mechanical properties of CaCu3Ti3.925(Nb0.5Al0.5)0.075O12 & Al reinforced epoxy-composites (0–3) for embedded capacitor applications

CaCu₃Ti_3.925(Nb_0.5Al_0.5)_0.075O₁₂ [CCTNAO] ceramics were synthesized by microwave assisted solid state reaction technique. CCTNAO ceramics possessed room temperature (RT) dielectric constant (ε_r) ～ 24,173 with tanδ ～0.149 at 1 kHz frequency. Commercially available epoxy-resin, hardener, Al-powder along with CCTNAO powder were used to prepare epoxy based 0–3 composites. Maximum ε_r ～33.37 with tanδ ～0.107 at RT were obtained for 40 vol% CCTNAO loading in epoxy. For x = 0.2 in (1-x)[0.8 Epoxy-0.2 CCTNAO]-x Al Epoxy composites, highest ε_r ～77.6 with tanδ ～ 0.15 at 1 kHz frequency were observed. Increase in ε_r with the increase of Al filler content in composites is attributed to interfacial polarization and cluster formations. Different theoretical models were discussed to explain the dielectric properties of synthesized composites. Experimentally measured values of ε_eff were in close agreement with EMT model (n = 0.13) and Yamada Model (η = 7). An empirical proposed power law ε_eff = ε_m(1+x)ⁿ, with n ～ 10 had a considerable agreement with the experimental results. Vickers hardness test study was carried out to ascertain the mechanical properties of the synthesized composites.     

Formation of Sn filled CNTs nanocomposite: Study of their magnetic,dielectric properties and enhanced microwave absorption performance at gigahertz frequencies

The Simplistic formation, advantageous configuration, non-colossal magnetoresistance and broadband absorption are important parameters for microwave absorbent materials. In this study, a core-shell nanocomposite comprising of Sn-filled carbon nanotubes (Sn/CNTs) was prepared by arc discharge method. The microstructure, morphology and surface composition of Sn/CNTs-based core-shell nanocomposites were characterized in detail. Sn/CNTs nanocomposite showed a magnetic signal due to the broken bonds and defects at interfaces in Sn/CNTs. The weak ferromagnetism was found to be helpful in improving magnetic permeability in the Sn/CNTs which confirms its role as a magnetic loss material under incident electromagnetic wave. Sn-filled CNTs revealed an appropriate value of dielectric constant, which plays an important role in impedance matching upon incident electromagnetic wave. The composite of Sn-CNTs and paraffin with a 50 wt % loading showed the lowest reflection loss (RL) of ?43.87 dB at 10 GHz, with a wide effective absorption band (RL ≤ ?10 dB) of 3 GHz in thickness of 2.3 mm. This enhanced performance is attributed to the combined effect of the conduction loss in one-dimensional core-shell architecture, the interfacial loss Sn-CNT interface, the magnetic loss due to defects-induced ferromagnetism in Sn shell, and in the carbon-containing atomic layers of CNTs.     

Effect of organic solvent on the cold sintering processing of SrFe12O19 platelet-based permanent magnets

In this work we have investigated the effect of the solvent during the processing of SrFe₁₂O₁₉ platelet-based permanent magnets by cold sintering process (CSP) plus a post-thermal treatment. Several organic solvents: glacial acetic acid, oleic acid and oleylamine have been analyzed, optimizing the CSP temperatures at 190?270 °C, under pressures of 375?670 MPa and 6?50 wt% of solvent. Modifications in the morphological and structural properties are identified depending on the solvent, which impacts on the magnetic response. Independently of the solvent, the mechanical integrity of ferrite magnets obtained by CSP is improved by a post-annealing at 1100 °C for 2 h, resulting in relative densities around 92 % with an average grain size of 1 μm and a fraction of SrFe₁₂O₁₉ phase >91 %. H_C ≥ 2.1 kOe and M_S of 73 emu/g are obtained in the final sintered ceramic magnets, exhibiting the highest H_C value of 2.8 kOe for the magnet sintered using glacial acetic acid.     

Impedance matching optimization of SiCf/Si3N4–SiOC composites for excellent microwave absorption properties

SiC fiber reinforced ceramic matrix composites (SiC_f-CMCs) are considered to be one of the most promising materials in the electromagnetic (EM) stealth of aero-engines, which is expected to achieve strong absorption and broad-band performance. Multiscale structural design was applied to SiC_f/Si₃N₄–SiOC composites by construction of micro/nanoscale heterogeneous interfaces and macro double-layer impedance matching structure. SiC_f/Si₃N₄–SiOC composites were fabricated by using SiC fibers with different conductivities and SiOC–Si₃N₄ matrices with gradient impedance structures to improve impedance matching effectively. Owing to its unique structure, SiC_f/Si₃N₄–SiOC composites (A3-composites) achieved excellent EM wave absorption performance with a minimum reflection coefficient (RC_min) of ?25.1 dB at 2.45 mm and an effective absorption bandwidth (EAB) of 4.0 GHz at 2.85 mm in X-band. Moreover, double-layer SiC_f/Si₃N₄–SiOC with an improved impedance matching structure obtained an RC_min of ?56.9 dB and an EAB of 4.2 GHz at 3.00 mm, which means it can absorb more than 90% of the EM waves in the whole X-band. The RC is less than ?8 dB at 2.6–2.8 mm from RT to 600 °C in the whole X-band, displaying excellent high-temperature absorption performance. The results provide a new design opinion for broad-band EM absorbing SiC_f-CMCs at high temperatures.     

(Cu1/3Nb2/3)4+ ionic substituting effects,low-temperature sintering behaviors,and improved temperature stability of Ba3Nb4Ti4O21 microwave dielectric ceramics

In this study, (Cu_1/3Nb_2/3)⁴⁺ complex cation and BaO–ZnO–B₂O₃ glass frit were adopted to solve the high sintering temperature and poor temperature stability of Ba₃Nb₄Ti₄O₂₁ ceramics. It is shown that pure Ba₃Nb₄Ti₄O₂₁ phase was formed when Ti site was partially replaced by (Cu_1/3Nb_2/3)⁴⁺ cation. The increasing number of dopants decreases the dielectric polarizability, correspondingly, the dielectric constant and temperature coefficient of the resonance frequency values are reduced consistently. The variation of the Q × f value is determined by internal ionic packing fraction and external sintering densification. The (Cu_1/3Nb_2/3)⁴⁺ cation effectively decreases the suitable sintering temperature from 1200 to 1050 °C while greatly improving the temperature stability. BaO–ZnO–B₂O₃ glass was used to further improve the low-temperature sintering characteristics of Ba₃Nb₄Ti₄O₂₁ ceramics. It is proven that the addition of glass frits effectively decreases the temperature to 925 °C with combinational excellent microwave dielectric properties: ε_r ～55.6, Q × f ～5700 GHz, τ_f ～3 ppm/^°C, making the Ba₃Nb₄Ti₄O₂₁ ceramics promising in the applications of low-temperature cofired ceramic technology.     

Microstructure and flexural strength of the Y:TZP/BG composite

The addition of bioactive glasses to a Y:TZP matrix represents a feasible alternative to provide bioactivity to this material and optimize osseointegration. This work evaluated the effect of the BG concentration (0 and 10 wt%) and the sintering temperature (1200°C and 1300°C) on the microstructure, relative density, and flexural strength of the composite Y:TZP/BG. The Y:TZP and Y:TZP/BG powders were uniaxially pressed and sintered at 1200°C or 1300°C for 1 h. The microstructure was characterized by X-ray diffraction analysis, scanning electron microscopy, and energy-dispersive X-ray Spectroscopy. Relative density was calculated from density values obtained using the Archimedes’ principle. For the flexural strength, specimens (n = 6) were fractured in a biaxial flexural setup using a piston-on-three-balls fixture in a universal testing machine. Bioactivity test was performed in simulated body fluid solution. The results suggested that BG addition decreased the grain size of the composite, increased porosity and caused a significant decrease in the relative density and flexural strength. Crystalline phases of calcium stabilized cubic zirconia and sodium zirconium silicate were formed after the addition of BG. Finally, it was concluded that composite specimens sintered at 1300°C showed the highest density values and larger grains compared to those sintered at 1200°C.