Processing of porous Ti and Ti5Mn foams by spark plasma sintering

Titanium and its alloys are one of the best metallic biomaterials to be used for implant application. In this study, porous Ti and Ti5Mn alloy with different porosities were successfully synthesized by powder metallurgy process with the addition of NH₄HCO₃ as space holder and TiH₂ as foaming agent. The consolidation of powder was achieved by spark plasma sintering process (SPS) at 16 MPa and pressureless conditions. The morphology of porous structure was investigated by using scanning electron microscopy (SEM) and X-ray micro-tomography (μ-CT). Nano-indentation tester was used to evaluate Young’s modulus of the porous Ti and Ti5Mn alloy. Experimental results showed that pure Ti sample, which sintered under pressure of 16 MPa, full relative density was achieved even at a relative low sintering temperature 750 °C; however, in the case of pressureless condition at sintering temperature 1000 °C the porosity was 53% and Young’s modulus was 40 GPa. The Ti5Mn alloy indicated a good pore distribution, and the porosity decreased from 56% to 21% by increasing the sintering temperature from 950 °C to 1100 °C. Young’s modulus was increased from 35 GPa to 51.83 GPa with increasing of the sintering temperatures from 950 °C to 1100 °C.     

Preparation and properties of unidirectional boron nitride fibre reinforced boron nitride matrix composites via precursor infiltration and pyrolysis route

The unidirectional boron nitride fibre reinforced boron nitride matrix (BN_f/BN) composites were prepared via the precursor infiltration and pyrolysis (PIP) route, and the structure, composition, mechanical and dielectric properties were studied. The composites have a high content and fine crystallinity of BN. The density is 1.60 g cm⁻³ with a low open porosity of 4.66%. The composites display good mechanical properties with the average flexural strength, elastic modulus and fracture toughness being 53.8 MPa, 20.8 GPa and 6.88 MPa m^1/2, respectively. Lots of long fibres pull-out from the fracture surface, suggesting a good fibre/matrix interface. As temperature increases, both of the flexural strength and elastic modulus exhibit a decreasing trend, with the lowest values being 36.2 MPa and 8.6 GPa at 1000 °C, respectively. The desirable residual ratios of the flexural strength and elastic modulus at 1000 °C are 67.3% and 41.3%, respectively. The composites have excellent dielectric properties, with the average dielectric constant and loss tangent being 3.07 and 0.0044 at 2-18 GHz, respectively.     

Effects of borosilicate glass addition on the structure and dielectric properties of ZnTiO3 ceramics

ZnTiO₃ powders and borosilicate glass were made by sol-gel method, and then mixed for co-firing at low temperatures. The results show that the borosilicate glass was liquefied to improve the density of the ceramic during sintering. However, Zn₄O(BO₂)₆ and TiO₂ were formed if too much borosilicate glass was added (over 10 wt.%). The microwave dielectric properties of the ZnTiO₃ co-fired with borosilicate glass were also improved dramatically. With 5 wt.% borosilicate glass addition, ZnTiO₃ ceramics can be sintered at 850 °C and shows excellent microwave properties: 22.2 for dielectric constant, and 52,460 for Q × f value at a frequency of 6 GHz.     

Preparation and dielectric properties of BaCu(B2O5)-doped SrTiO3-based ceramics for energy storage

BaCu(B₂O₅) (BCB) was used as sintering aids to lower the sintering temperature of multi-ions doped SrTiO₃ ceramics effectively from 1300 °C to 1075 °C by conventional solid state method. The effect of BCB content on crystalline structures, microstructures and properties of the ceramics was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and dielectric measurements, respectively. The addition of BCB enhanced the breakdown strength (BDS) while did not sacrifice the dielectric constant. The enhancement of BDS should be due to the modification of microstructures, i.e., smaller and more homogeneous grain sizes after BCB addition. The dielectric constant of BCB-doped ceramics maintained a stable value with 1.0 mol% BCB, which was dominated by the combination of two opposite effects caused by the presence of second phases and the incorporation of Cu²⁺ and Ba²⁺, while further increase was owing to the increase of dissolved Ba²⁺ ions when the content of BCB is more than 2.0 mol%. The multi-ions doped SrTiO₃ ceramics with 1.0 mol% BCB addition showed optimal dielectric properties as follows: dielectric constant of 311.37, average breakdown strength of 28.78 kV/mm, discharged energy density of 1.05 J/cm³ and energy efficiency of 98.83%.     

Microwave dielectric properties and microstructures of CuO- and ZnO-doped LaAlO3 ceramics

The microwave dielectric properties and the microstructures of 0.25 wt.% CuO-doped LaAlO₃ ceramics with ZnO additions have been investigated. The sintered LaAlO₃ ceramics are characterized by X-ray diffraction spectra and scanning electron microscopy (SEM). Tremendous reduction in sintering temperature can be achieved with the addition of sintering aids CuO and ZnO. The ceramic samples show that dielectric constants (ε_r) of 22−24 and Q×f values of 33,000−57,000 (at 9.7 GHz) can be obtained at low sintering temperatures 1340−1460°C. The temperature coefficient of resonant frequency varies from −24 to −48 ppm/°C. At the level of 0.25 wt.% CuO and 1 wt.% ZnO additions, LaAlO₃ ceramics possesses a dielectric constant (ε_r) of 23.4, a Q×f value of 57,000 (at 9.7 GHz) and a τ_f value of −38 ppm/°C at 1400°C for 2 h.     

Effect of phosphorus addition on the sintering and dielectric properties of Pb(Zr0.52Ti0.48)O3

It has been found that the sintering temperature of piezoelectric Pb(Zr_0.52Ti_0.48)O₃ (PZT) can be reduced by phosphorus addition without compromising the dielectric properties. A sintered density of 98.6% of the theoretical density was obtained for 2 wt.% P₂O₅ addition after sintering at 1050 °C for 4 h. The P₂O₅ addition, either above or below 2 wt.%, showed an inferior densification. Coincidentally, the P₂O₅ addition gave rise to a lower lead loss, and the dielectric constant showed a peak at 1 wt.% P₂O₅ addition.     

Characterization and dielectric behavior of CuO-doped ZnTa2O6 ceramics at microwave frequency

The effects of CuO addition on the microstructures and microwave dielectric properties of ZnTa₂O₆ ceramics were investigated. CuO was selected as a liquid-phase sintering aid to lower the sintering temperature of ZnTa₂O₆ ceramics. With CuO addition, the sintering temperature of ZnTa₂O₆ can be effectively reduced from 1350 to 1230 °C. The crystalline phase exhibited no phase difference and no second phase was detected at low addition levels (0.25-1 wt.%). The quality factors Q × f were strongly dependent upon the CuO concentration. A Q × f value of 65,500 GHz was obtained for specimen with 0.25 wt.% CuO addition at 1230 °C. For all levels of CuO concentration, the relative dielectric constants were not significantly different and ranged from 34.2 to 35.7. Tunable temperature coefficient of resonant frequency (τ_f) can be adjusted to zero by appropriately turning the CuO content.     

Improved high-Q microwave dielectric resonator using CuO-doped MgNb2O6 ceramics

The microwave dielectric properties and the microstructures of MgNb₂O₆ ceramics with CuO additions (1-4 wt.%) prepared with conventional solid-state route have been investigated. The sintered samples exhibit excellent microwave dielectric properties, which depend upon the liquid phase and the sintering temperature. It is found that MgNb₂O₆ ceramics can be sintered at 1140 °C due to the liquid phase effect of CuO addition. At 1170 °C, MgNb₂O₆ ceramics with 2 wt.% CuO addition possesses a dielectric constant (ε_r) of 19.9, a Q×f value of 110,000 (at 10 GHz) and a temperature coefficient of resonant frequency (τ_f) of −44 ppm/°C. The CuO-doped MgNb₂O₆ ceramics can find applications in microwave devices requiring low sintering temperature.     

Low temperature sintering and microwave dielectric properties of SmAlO3 ceramics

The effects of sintering aids on the microstructures and microwave dielectric properties of SmAlO₃ ceramics were investigated. CuO and ZnO were selected as sintering aids to lower the sintering temperature of SmAlO₃ ceramics. With the additions, the sintering temperature of SmAlO₃ can be effectively reduced from 1650 to 1430°C. The crystalline phase exhibited no phase differences at low addition level while Sm₄Al₂O₉ appeared as a second phase as the doping level was over 0.5 wt.%. In spite of the additions, the dielectric constants showed no significant change and ranged 19-21. However, the quality factor Q×f was strongly dependent upon the type and amount of additions. The Q×f values of 51,000 and 41,000 GHz could be obtained at 1430°C with 0.25 wt.% CuO and ZnO additions, respectively. The temperature coefficients depended on the additions and varied from −40 to −65 ppm/°C. Results of X-ray diffractions, EDS analysis and scanning electron microscopy were also presented.     

Microwave dielectric properties and microstructures of the 11Li2O-3Nb2O5-12TiO2 ceramics with B2O3 addition

The effects of B₂O₃ addition, as a sintering agent, on the sintering behavior, microstructure and microwave dielectric properties of the 11Li₂O-3Nb₂O₅-12TiO₂ (LNT) ceramics have been investigated. With the low-level doping of B₂O₃ (≤2 wt.%), the sintering temperature of the LNT ceramic could be effectively reduced to 900 °C. The B₂O₃-doped LNT ceramics are also composed of Li₂TiO₃ss and “M-phase” phases. No other phase could be observed in the 0.5-2 wt.% B₂O₃-doped ceramics sintered at 840-920 °C. The addition of B₂O₃ induced no obvious degradation in the microwave dielectric properties but increased the τ_f values. Typically, the 0.5 wt.% B₂O₃-doped ceramics sintered at 900 °C have better microwave dielectric properties of ?_r = 49.2, Q × f = 8839 GHz, τ_f = 57.6 ppm/°C, which suggest that the ceramics could be applied in multilayer microwave devices requiring low sintering temperatures.     

Influence of Bi2O3 and CuO addition on low-temperature sintering and dielectric properties of Ba0.6Sr0.4TiO3 ceramics

In this study, we tried to lower the sintering temperature of Ba_0.6Sr_0.4TiO₃ (BST) ceramics by several kinds of adding methods of Bi₂O₃, CuO and CuBi₂O₄ additives. The effects of different adding methods on the microstructures and the dielectric properties of BST ceramics have been studied. In the all additive systems, the single addition of CuBi₂O₄ was the most effective way for lowering the sintering temperature of BST. When CuBi₂O₄ of 0.6 mol% was mixed with starting BST powders and sintered at 1100 °C, the derived ceramics demonstrated dense microstructure with a low dielectric constant (? = 4240), low dielectric loss (tan δ = 0.0058), high tunability (Tun = 38.3%) and high Q value (Q = 251). It was noteworthy that the sintering temperature was significantly lowered by 350 °C compared with no-additive system, and the derived ceramics maintained the excellent microwave dielectric properties corresponding to pure BST.     

Effect of sintering temperature on dielectric properties of Ba0.6Sr0.4TiO3–MgO composite ceramics prepared from fine constituent powders

Composite ceramics of Ba_0.6Sr_0.4TiO₃ + 60 wt.% MgO were prepared from fine constituent powders by sintering at 1200–1280 °C. The composite specimens sintered at the relatively low temperatures showed satisfactory densification due to fine morphology of the constituent powders. The elevation of sintering temperature promoted the incorporation of Mg²⁺ into the lattice of the Ba_0.6Sr_0.4TiO₃ phase and grain growth of the two constituent phases. The dependence of the dielectric properties on sintering temperature was explained in relation to the structural evolution. Controlling the sintering temperature of the composite was found to be important to achieve the desired nonlinear dielectric properties. Sintering at 1230 °C was determined to be preferred for the composite in terms of the nonlinear dielectric properties. The specimen sintered at the temperature attained a tunability of 17.3% and a figure of merit of 127 at 10 kHz and 20 kV/cm.     

Effect of liquid-forming additives on the sintering and mechanical properties of Al2O3/3Y-TZP (30 vol.%) composite

Al₂O₃/3Y-TZP (30 vol.%) composite was pressurelessly sintered with addition of TiO₂MnO₂ and/or CaOAl₂O₃SiO₂ glass. It was found that TiO₂MnO₂ addition greatly enhanced the densification of the composite by the formation of a low-viscosity liquid at sintering temperature. In contrast, the high-viscosity liquid formed by CaOAl₂O₃SiO₂ glass improved mechanical properties because of its repressing effect on grain growth. The composite could be obtained at a temperature as low as 1400°C by co-doping with TiO₂MnO₂ and CAS glass. Bending strength of 552±64 MPa and fracture toughness of 6.03±0.22 MPa m^1/2 were obtained with a doping level of 2 wt.% TiO₂MnO₂ and 2 wt.% CAS glass.     

Low-temperature sintering of (Zn0.8 Mg0.2)2SiO4-TiO2 ceramics

Effect of Li₂O-B₂O₃-SiO₂ (LBS) glass on the sintering behavior and the microwave dielectric properties of (Zn_0.8 Mg_0.2)₂SiO₄-TiO₂ (ZMST) ceramics were investigated. The Li₂O-B₂O₃-SiO₂ glass lowered the sintering temperature of ZMST ceramics effectively from 1250 to 870 °C. The unknown second phase, which was formed in the ZMST ceramics increased with the addition of LBS glass. With increasing the LBS glass content, the bulk density, dielectric constant (ε_r) and the maximum Q × f value decreased, and the temperature coefficient of resonant frequency (τ_f) shifted to a negative value. (Zn_0.8 Mg_0.2)₂SiO₄-TiO₂ ceramics with 3 wt.% Li₂O-B₂O₃-SiO₂ glass sintered at 870 °C for 2 h shows excellent dielectric properties: ε_r = 8.48, Q × f = 11500 GHz, and τ_f = 0 ppm/°C.     

Improved mechanical property of foam glass composites toughened by glass fiber

The mechanically improved foam glass composite toughened by glass fiber was prepared by sintering technique, using waste sodium-calcium silicon flat glass powder as main raw materials. In this study, the preparation and properties of the samples were characterized by differential thermal analysis (DTA), field-emission scanning electron microscopy (FESEM) and mechanical property test. The specific strength of the composite was defined for the first time, and applied into the investigation of mechanical property. The results show that the specific improved bending strength of 10.45-22.26 MPa/(g cm^− 3), and the specific compressive strength of 30.45-34.34 MPa/(g cm^− 3) can be displayed when sintered at 790-815 °C with the addition of 5-25 wt.% glass fiber. Good correlations between the microstructure (in particular the fiber distribution), the high specific strength and the high modulus of elasticity of glass fibers.     

Study on properties of BaxSmyTi7O20 ceramics with CaO-SiO2-B2O3 glass

The effect of CaO-SiO₂-B₂O₃ (CSB) glass addition on the sintering temperature and dielectric properties of Ba_xSm_yTi₇O₂₀ ceramics has been investigated using X-ray diffraction, scanning electron microscopy and differential thermal analysis. The CSB glass starts to melt at about 970 °C, and a small amount of CSB glass addition to Ba_xSm_yTi₇O₂₀ ceramics can greatly decrease the sintering temperature from about 1350 to about 1260 °C, which is attributed to the formation of liquid phase. It is found that the dielectric properties of Ba_xSm_yTi₇O₂₀ ceramics are dependent on the amount of CSB glass and the microstructures of sintered samples. The product with 5 wt% CSB glass sintered at 1260 °C is optimal in these samples based on the microstructure and the properties of sintering product, when the major phases of this material are BaSm₂Ti₄O₁₂ and BaTi₄O₉. The material possesses excellent dielectric properties: ?_r = 61, tan δ = 1.5 × 10⁻⁴ at 10 GHz, temperature coefficient of dielectric constant is −75 × 10⁻⁶ °C⁻¹.     

Effect of ZnO addition on the sintering and electrical properties of (Mn,W)-doped PZT-PMS-PZN ceramics

The effect of ZnO addition on the phase structure, microstructure and dielectric and piezoelectric properties of 0.2 wt.% MnO₂ and 0.6 wt.% WO₃-doped Pb(Zr_0.52Ti_0.48)O₃-Pb(Mn_1/3Sb_2/3)O₃-Pb(Zn_1/3Nb_2/3)O₃ (PZT-PMS-PZN) ceramics was investigated. X-ray diffraction shows that the phase structure of ceramics is transformed from rhombohedral to tetragonal with the increasing of ZnO addition. The bulk density significantly increases when ZnO is added and then it slightly decreases for ZnO addition above 0.2 wt.%. SEM micrographs show the grains of ceramics are uniform and well developed by adding 0.1 wt.% ZnO. The Curie temperature (T_c) of 270 °C is obtained at the 0.1 wt.% ZnO addition. Mechanical quality factor (Q_m), electromechanical coupling factor (K_p) and piezoelectric constant (d₃₃) increase firstly, and then decrease with the increasing of ZnO addition, while dielectric loss tan δ drops all the time. The Q_m, K_p, d₃₃, tan δ and T_c of the ceramics show the optimum values of 1899, 0.55, 300 (pC/N), 0.0063 and 270 °C, respectively, at the lower sintering temperature of 1120 °C and with 0.1 wt.% ZnO addition.     

Low permittivity SrCuSi4O10-LMZBS glass composite for LTCC applications

The tetragonal gillespite type SrCuSi₄O₁₀ (SCS) was prepared by the conventional solid-state ceramic route. The SCS sintered at 1100 °C/6 h showed ε_r = 4.0 and tan δ = 1.1 × 10⁻³ at 5 GHz. The SCS has poor sinterability and the addition of lithium magnesium zinc borosilicate glass (20: Li₂O, 20: MgO, 20: ZnO, 20: B₂O₃, 20: SiO₂) lowered the sintering temperature and improved densification. The SCS ceramic with 5 wt.% LMZBS glass sintered at 900 °C has ε_r = 5.0 and tan δ = 1.9 × 10⁻³ at 5 GHz. The composite is chemically compatible with the common electrode material silver.     

Sintering and dielectric properties of 0.88Al2O3-0.12TiO2 microwave ceramics by glass addition

The microwave characteristics and the microstructures of 0.88Al₂O₃-0.12TiO₂ with various amounts of MgO-CaO-SiO₂-Al₂O₃ (MCAS) glass sintered at different temperatures have been investigated. The sintering temperature can be lowered to 1300 °C by the addition of MCAS glass. The densities, dielectric constants (ε_r) and quality values (Q×f) of the MCAS-added 0.88Al₂O₃-0.12TiO₂ ceramics decrease with the increase of MCAS glass content. The temperature coefficients of the resonant frequency (τ_f) are shifted to more negative values as the MCAS content or the sintering temperatures increase. The change of the crystalline phases of Al₂TiO₅ phase and rutile-TiO₂ phase has profound effects on the microwave dielectric properties of the MCAS-added Al₂O₃-TiO₂ ceramics. As sintered at 1250 °C, 0.88Al₂O₃-0.12TiO₂ ceramics with 2 wt.% MCAS glass addition exists a ε_r value of 8.63, a Q×f value of 9578 and a τ_f value of +5 ppm/°C.     

Microwave dielectric and elastic properties of glass-added Ba6−3xR8+2xTi18O54 (x = 2/3)

Microwave dielectric properties of Ba_6−3xSm_8+2xTi₁₈O₅₄ (x = 2/3) [BST] ceramics with the addition of 0–3 wt.% of various glasses have been studied. It has been found that the addition of 0.5 wt.% of the glasses decreases the sintering temperature by about 150 °C. In general, addition of 0.5 wt.% of Zn, Mg and Pb-based glasses deteriorate the quality factor, whereas aluminum and barium borosilicates do not decrease it considerably. The quality factor and dielectric constant decrease with increasing amount of glass. The temperature coefficient of resonant frequency shifts towards positive or negative depending on the composition of the glass. A glass–ceramic composite with a dielectric constant 64, Q × f nearly 8500 GHz and near to zero τ_f could be obtained at a sintering temperature of 1175 °C when 3–4 wt.% Al₂O₃–B₂O₃–SiO₂ glass was added to BST ceramic. The Young's modulus decreases with increasing amount of glass, irrespective of the composition of glass.