Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

B4C-TiB2复相陶瓷的强韧化研究

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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.     

Microstructure–mechanical properties relations in SiC–TiB2 composite

Densification and mechanical properties (fracture toughness, flexural strength and hardness) of SiC–TiB₂ composite were studied. Pressureless sintering experiments were carried out on samples containing 0–50 vol% of TiB₂ created by in situ reaction between TiO₂, B₄C and carbon. Al₂O₃ and Y₂O₃ were used as sintering additives to create liquid phase and promote densification at sintering temperature of 1940 °C. The sintered samples were subsequently heat treated at 1970 °C. It was found that the presence of TiB₂ serves as an effective obstacle to SiC grain growth as well as crack propagation thus increasing both strength and fracture toughness of sintered SiC–TiB₂ composite. The subsequent heat treatment of sintered samples promoted the elongation of SiC matrix and further improved mechanical properties of the composite. The best mechanical properties were measured in heat-treated samples containing 12–24 vol% TiB₂. The maximum flexural strength of ∼600 MPa was obtained in samples with 12 vol% TiB₂ whereas the maximum fracture toughness of 6.6 MPa m^1/2 was obtained in samples with 24 vol% TiB₂. Typical microstructures of samples with the mentioned volume fractions of TiB₂ consist of TiB₂ particles (<5 μm) uniformly dispersed in a matrix of elongated SiC plates.     

Effects of sintering parameters on the microstructure and tensile properties of in situ TiBw/Ti6Al4V composites with a novel network architecture

In order to better understand the relationship of processing–structure–mechanical properties of in situ TiB whisker reinforced Ti6Al4V (TiBw/Ti64) composites with a novel network architecture, the effects of sintering parameters on the microstructure and tensile properties of the composites were investigated. TiB whiskers with the highest aspect ratio and the coarsest whiskers were obtained at 1100 °C and 1200 °C due to the skips of whisker growth speeds along the [0 1 0] direction and the [0 0 1] and [1 0 0] directions, respectively. Additionally, TiB whisker with a claw-like structure can be synthesized from one TiB₂ polycrystal parent. The quasi-continuous network architecture of TiBw/Ti64 composites can be achieved at higher sintering temperatures more than 1200 °C. The prepared composites with the quasi-continuous network architecture exhibit a superior combination of tensile properties.     

Optimization of deposition temperature and atmosphere for pulsed laser deposited Sr2FeMoO6 thin films

Double perovskite Sr₂FeMoO₆ films were deposited by pulsed laser deposition at a wide temperature range and different atmospheres. The best films with T_C = 340-370 K and low temperature magnetization of around 2.2 μ_B/f.u. were deposited at 1050 °C with 9 Pa Ar/5%H₂ atmosphere. X-ray diffraction showed no impurities and full texturization of all the films. Atomic force microscopy revealed increasing surface roughness with increasing deposition temperature.     

Low temperature sintering and microwave dielectric properties of ZnTiNb2O8 ceramics with BaCu(B2O5) additions

The phases, microstructure and microwave dielectric properties of ZnTiNb₂O₈ ceramics with BaCu(B₂O₅) additions prepared by solid-state reaction method have been investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The pure ZnTiNb₂O₈ ceramic shows a high sintering temperature of about 1250 °C. However, it was found that the addition of BaCu(B₂O₅) lowered the sintering temperature of ZnTiNb₂O₈ ceramics from above 1250 °C to 950 °C due to the BCB liquid-phase. The results showed that the microwave dielectric properties were strongly dependent on densification, crystalline phases and grain size. Addition of 3 wt% BCB in ZnTiNb₂O₈ ceramics sintered at 950 °C afforded excellent dielectric properties of ?_r = 32.56, Q × f = 20,100 GHz (f = 5.128 GHz) and τ_f = −64.87 ppm/°C. These represent very promising candidates for LTCC dielectric materials.     

The mechanism of thermal explosion (TE) synthesis of TiC-TiB2 particulate locally reinforced steel matrix composites from an Al-Ti-B4C system via a TE-casting route

TiC-TiB₂ particulate locally reinforced steel matrix composites were fabricated by a novel TE-casting route from an Al-Ti-B₄C system with various B₄C particle sizes. The formation mechanism of TiC and TiB₂ in the locally reinforced regions was investigated. The results showed that TiC and TiB₂ are formed and precipitated from Al-Ti-B-C melt resulting from the dissociation of B₄C into Al-Ti melt when the concentrations of B and C atoms in the Al-Ti-B-C melt become saturated. However, in the case of coarse B₄C powders (≥40 μm) used, the primary reaction in the Al-Ti-B-C melt is quite limited due to the poor dissociation of B₄C. The poured steel melt infiltrates into the primary reaction product and thus leads to the formation of Al-Fe-Ti-B-C melt, thanks to the favorable reaction of molten Fe with remnant B₄C, and then TiC and TiB₂ are further formed and precipitated from the saturated Al-Fe-Ti-B-C melt. The relationship between the mechanisms of thermal explosion (TE) synthesis of TiC and TiB₂ in the electric resistance furnace and during casting was proposed.     

Formation of TiB2 by volume combustion and mechanochemical process

Titanium diboride was produced both by volume combustion synthesis (VCS) and by mechanochemical synthesis (MCP) through the reaction of TiO₂, B₂O₃ and Mg. VCS products, expected to be composed of TiB₂ and MgO, were found to contain also side products such as Mg₂TiO₄, Mg₃B₂O₆, MgB₂ and TiN. HCl leaching was applied to the reaction products with the objective of removing MgO and the side products. Formation of TiN could be prevented by conducting the VCS under an argon atmosphere. Mg₂TiO₄ did not form when 40% excess Mg was used. Wet ball milling of the products before leaching was found to be effective in removal of Mg₃B₂O₆ during leaching in 1 M HCl. When stoichiometric starting mixtures were used, all of the side products could be removed after wet ball milling in ethanol and leaching in 5 M HCl when pure TiB₂ was obtained with a molar yield of 30%. Pure TiB₂ could also be obtained at a molar yield of 45.6% by hot leaching of VCS products at 75 °C in 5 M HCl, omitting the wet ball milling step. By MCP, products containing only TiB₂ and MgO were obtained after 15 h of ball milling. Leaching in 0.5 M HCl for 3 min was found to be sufficient for elimination of MgO. Molar yield of TiB₂ was 89.6%, much higher than that of VCS. According to scanning electron microscope analyses, the TiB₂ produced had average grain size of 0.27 ± 0.08 μm.     

Low-temperature sintering and compatibility with silver electrode of Ba4MgTi11O27 microwave dielectric ceramic

Ba₄MgTi₁₁O₂₇ microwave dielectric ceramic was investigated using X-ray diffraction, scanning electron microscopy and dielectric measurement. The pure Ba₄MgTi₁₁O₂₇ ceramic shows a high sintering temperature (∼1275 °C) and good microwave dielectric properties as Q × f of 19,630 GHz, ?_r of 36.1, τ_f of 14.6 ppm/°C. It was found that the addition of BaCu(B₂O₅) (BCB) can effectively lower the sintering temperature from 1275 to 925 °C, and does not induce much degradation of the microwave dielectric properties. The BCB-doped Ba₄MgTi₁₁O₂₇ ceramics can be compatible with Ag electrode, which makes it a promising ceramic for LTCC technology application.     

Electrical discharge machining of ZrO2 toughened WC composites

The interrelationships between the dispersion of the ZrO₂ phase and the electrical discharge machining (EDM) behaviour of WC based composites with 0, 5 or 10 vol% of ZrO₂ are investigated. Special attention was given to the homogeneity of the ultrafine WC – nanometric ZrO₂ powder based composites which were fully densified by means of pulsed electric current sintering (PECS). X-ray photoelectron spectroscopy (XPS) measurements revealed the presence of a nanometric WO₃ layer on the EDM surface, confirming oxidation as the major material removal mechanism (MRM). The surface roughness after the final EDM finishing regime was strongly influenced by the composite homogeneity and could be reduced down to 0.15 μm (R_a) on agglomerate-free composites. Residual stress measurements indicated that EDM did not introduce a significant amount of surface stresses, especially not after the final finishing regime. XRD measurements of EDM surfaces however indicated surface depletion of ZrO₂ by the formation of ZrC and W₂C during spark erosion.     

Reciprocal sliding wear behaviour of B4C particulate reinforced aluminum alloy composites

Aluminum based composites reinforced with B₄C particles were prepared by cryomilling and subsequent hot pressing steps. The cryomilled powders dispersed with 5 wt.% or 10 wt.% B₄C particles were hot pressed under a pressure of 600 MPa at 350 °C. Microstructural studies conducted on the composites indicated that homogeneous distribution of the B₄C particles in the Al matrix and a good interface between them had been achieved. According to the results of reciprocating wear tests carried out by utilizing alumina and steel balls, wear resistance increased with increasing B₄C particle content.     

SiC matrix composites reinforced with internally synthesized TiB2

A new process of preparing particulate-reinforced ceramic composites by internal synthesis has been developed. SiC powder mixed with TiN and amorphous boron was hot-pressed above 2000° C in an argon atmosphere. The boron molar content in the mixture was designed to be more than twice that of TiN. In the process of hot-pressing, the following reaction took place between 1100 and 1700° C TiN+2B TiB₂+1/2N₂ The synthesis of TiB₂ was followed by the densification of SiC matrix with the aid of the excess boron. The new process provides SiC matrix composites in which fine TiB₂ particulates are dispersed. Compared with hot-pressed monolithic SiC, the composite containing 20 vol % TiB₂ exhibits a 80% increase in fracture toughness and about the same flexural strength of 490 MPa at 20° C in air and 750 MPa at 1400° C in a vacuum.     

A simple synthesis route for high quality BaFe12O19 magnets

The present investigation reports the detailed analysis of the influence of B₂O₃-doping on magnetic and structural properties of hexagonal barium ferrites (BaFe₁₂O₁₉) synthesized via conventional ceramic technique. The results show that crystalline structure of barium ferrite is improved with small amounts of B₂O₃ between 0.1 and 1.0 wt%. Single phase particles has been obtained by 1.0 wt% B₂O₃-doping with calcination at temperatures as low as 850 °C and a range of boron concentration and calcination temperature has been extended in order to find the best synthesis conditions. Optimal properties have been achieved by 0.2 wt% of B₂O₃-doping and calcination at 1000 °C. The remanence and the saturation magnetizations increase considerably by about 40% in magnitude with B₂O₃.     

Improvements in mechanical properties of TiB2 by the dispersion of B4C particles

Densities up to 99% of the theoretical value were achieved by hot-pressing of TiB₂-B₄C composites at 1700° C for 1 h using 1 vol % Fe as a sintering aid. The microstructure consists of dispersed B₄C particles in a fine-grained TiB₂ matrix. Addition of B₄C particles increases the fracture toughness of TiB₂ (to 7.6 MPa m^1/2 at 20 vol % B₄C) and yields high fracture strength (to 700 MPa at 10 vol % B₄C). Microstructural observations indicate that the improved strength is a result of a higher density, smaller grain size and intergranular fracture, and the toughness increase is a result of crack deflection around the B₄C particles.     

Densification process of TaC/TaB2 composite in spark plasma sintering

A TaC composite with ∼11 wt% in situ TaB₂ was fabricated by spark plasma sintering at 1600–1900 °C. The densification process was studied by analysis of the densifying shrinkage of the powder compacts. Three distinct stages for densification were determined. The starting powder mixture of TaC, B₄C and Ta completed reaction to form the desired TaC and TaB₂ at temperature <1583 °C. At around ∼1750 °C, the TaC/TaB₂ material significantly improved relative density to ∼95% with rapid grain growth. The final densification took place very rapidly at 1900 °C by releasing a high pressure vapor.     

Low temperature extrusion of 6061 aluminum matrix composite reinforced with SnO2-coated Al18B4O33 whisker

The 6061 aluminum matrix composite reinforced with SnO₂-coated Al₁₈B₄O₃₃ whisker was fabricated by squeeze casting and following by extrusion extruded at elevated temperatures from 300 °C to 400 °C. Optimization of the extruding process, microstructure, texture and mechanical properties of the extruded composites were investigated. The lowest extrusion temperature at which a composite rod with high surface quality was successfully produced was 300 °C. The yield strength of composites is much improved after extrusion, and especially their elongation is increased by 300%. Such big improvements depend on a fact that SnO₂ coating can introduce low-melting-point Sn phase into the interface through an interfacial reaction. The melting of interphase and their surrounding areas is the main reason for the excellent extrusion ability of the composite. Besides, detailed X-ray diffraction analysis of the extruded composite textures reveals the significant effects of extrusion temperatures on their features.     

Reaction sintering fabrication of (AlN, TiN)-Al2O3 composite

The (AlN, TiN)-Al₂O₃ composites were fabricated by reaction sintering powder mixtures containing 10-30 wt.% (Al, Ti)-Al₂O₃ at 1420-1520°C in nitrogen. It was found that the densification and mechanical properties of the sintered composites depended strongly on the Al, Ti contents of the starting powder and hot pressing parameters. Reaction sintering 20 wt.% (Al, Ti)-Al₂O₃ powder in nitrogen in 1520°C for 30 min yields (AlN, TiN)-Al₂O₃ composites with the best mechanical properties, with a hardness HRA of 94.1, bending strength of 687 MPa, and fracture toughness of 6.5 MPa m^1/2. Microstructure analysis indicated that TiN is present as well dispersed particulates within a matrix of Al₂O₃. The AlN identified by XRD was not directly observed, but probably resides at the Al₂O₃ grain boundary. The fracture mode of these composites was observed to be transgranular.     

Effect of B2O3-Bi2O3-SiO2-ZnO glass on the sintering and microwave dielectric properties of 0.83ZnAl2O4-0.17TiO2

The 0.83ZnAl₂O₄-0.17TiO₂ (ZAT) ceramics were synthesized by solid state ceramic route. The effect of 27B₂O₃-35Bi₂O₃-6SiO₂-32ZnO (BBSZ) glass on the microwave dielectric properties of ZAT was investigated. The crystal structure and the microstructure of the ceramic-glass composites were studied by X-ray diffraction and scanning electron microscopic techniques. The low frequency dielectric loss was measured at 1 MHz. The dielectric properties of the sintered samples were measured in the microwave frequency range by the resonance method. Addition of 0.2 wt% of BBSZ improved the dielectric properties with quality factor (Q_u × f) > 120,000 GHz, temperature coefficient of resonant frequency (τ_f) = −7.3 ppm/°C and dielectric constant (?_r) = 11.7. Addition of 10 wt% of BBSZ lowered the sintering temperature to about 950 °C with Q_u × f > 10,000 GHz, ?_r = 10 and τ_f = −23 ppm/°C. The reactivity of 10 wt% BBSZ added ZAT with silver was also studied. The results show that ZAT doped with suitable amount of BBSZ glass is a possible material for low-temperature co-fired ceramic (LTCC) application.     

Synthesis of TiB2 powder from a mixture of TiN and amorphous boron

TiB₂ powder was synthesized by solid state reaction using amorphous boron and TiN as a source of titanium. The TiB₂ formation did not occur at all in a nitrogen atmosphere even at 1400° C. TiB₂ formed above 1100° C in argon and hydrogen atmospheres. The only crystalline phase of TiB₂ powder was favourably synthesized at 1400° C for 360 min in an argon atmosphere from a starting powder with a composition containing excess boron (B/Ti = 2.2). The synthesized powder was well dispersed and had a particle size of 0.5 to 2 µm. The powder activity was evaluated by sintering at 4 G Pa and 1300 to 1600° C for 15 min.