B4C-TiB2复相陶瓷的强韧化研究

采用热压烧结工艺，制备Ｂ４Ｃ－ＴｉＢ２复相陶瓷。结果表明，复相陶瓷的抗弯强度，断裂韧性和显向硬度受第二相ＴｉＢ２颗粒的影响，其中Ｂ４Ｃ－３０ｖｏｌ％ＴｉＢ２材料的弯曲强度为７２５ＭＰａ，比单体Ｂ４Ｃ提高６５％，Ｂ４Ｃ－４５ｖｏｌ＾ＴｉＢ２材料的断裂韧性为６．７ＭＰａ．ｍ＾１／２，比单体Ｂ４Ｃ提高８４％，由Ｂ４Ｃ基体和ＴｉＢ２颗粒热膨胀系数不匹配导致的残余应国是Ｂ４Ｃ－Ｔdisplay status     

Fabrication and thermal shock resistance of HfB2-SiC composite with B4C additives

A HfB₂ based ceramic matrix composite containing 20 vol.% SiC particles with 2 vol.% B₄C as sintering additives was fabricated by hot-pressed sintering. The microstructure and properties, especially the thermal shock resistance of the composite were investigated. Results showed that the addition of B4C improved the powder sinterability and led to obtaining nearly full dense composite. The flexural strength and fracture toughness of the composite were 771 MPa and 7.06 MPam^1/2, respectively. The thermal shock resistance tests indicated that the residual strength decreased significantly when the thermal shock temperature difference was higher than 600 °C. The large number of microcracks on the sample surface was the main reason for the catastrophic failure.     

In situ reacted TiB2-reinforced mullite

In situ formation of TiB₂ in mullite matrix through the reaction of TiO₂, boron and carbon has been studied. In hot-pressed and pressureless-sintered samples, in addition to TiB₂, TiC was also found to be dispersed phases in mullite matrix. However, in the case of pressurelesssintered samples, mullite/TiB₂ composite with 98% relative density can be obtained through a preheating step held at 1300 °C for longer than 3 h and then sintering at a temperature above 1600 °C. Hot-pressed composite containing 30 vol% TiB₂ gives a flexural strength of 427 MPa and a fracture toughness of 4.3 MPam^1/2. Pressureless-sintered composite containing 20 vol% TiB₂ gives a flexural strength of 384 MPa and a fracture toughness of 3.87 MPam^1/2.     

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.     

Mechanical properties of reaction sintered TiN ceramics with B4C addition

Reaction sintering of TiN with B₄C addition was developed to densify the composite without the application of external pressure. The process utilizes high affinity of B for Ti which leads to the formation of extremely fine highly active TiB₂. The addition of 6–8 wt% B₄C is sufficient to increase the sintered density to over 96% theoretical density, fracture toughness to 3.5 MPa·m^1/2, flexural strength to 415 MPa, and hardness to 14 GPa. The major toughening mechanism was identified to be the crack deflection caused by the presence of hard and tough TiB₂ particles. The large improvements in mechanical properties make this in situ produced composite viable material for applications requiring higher level of reliability.     

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.     

Densification behaviour and mechanical properties of pressureless-sintered B4C–CrB2 ceramics

B₄C based ceramics composites with 0–25 mol% CrB₂ were fabricated by pressureless sintering in the temperature range 1850°C to 2030°C. The CrB₂ addition enhanced the densification of B₄C due to the CrB₂–B₄C eutectic liquid phase formation. Both a high strength of 525 MPa and a modest fracture toughness of 3.7 MPa m^1/2 were obtained for the B₄C–20 mol% CrB₂ composite with a high-relative density of 98.1% after sintering at 2030°C. The improvement in fracture toughness is thought to result from the formation of microcracks and the deflection of propagating cracks resulting from the thermal expansion mismatch of CrB₂ and B₄C.     

Microstructure and mechanical properties of yttria-stabilized tetragonal zirconia polycrystals containing dispersed TiC particles

The microstructure and mechanical properties of hot-pressed yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) ceramics containing up to 30 vol % TiC particles were studied. Adding TiC particles to Y-TZP improved the bending strength and fracture toughness. With 20 vol% TiC particles the maximum bending strength and fracture toughness reached 1073±30.4 MPa and 14.56±0.25 MPa m^1/2, respectively. The residual tensile stress induced by the thermal expansion difference between ZrO₂ and TiC must have inhibited the tetragonal-monoclinic transformation. The stress-induced phase transformation was therefore not the dominant toughening mechanism. High-densities of dislocations within TiC particles and microcracking were detected by TEM. The improved toughness of the materials is considered to be the result of crack deflection, crack bowing of TiC particles and microcracking toughening of ZrO₂.     

Processing and Mechanical Properties of Boron Carbide–Titanium Diboride Ceramic Matrix Composites

The objective of the present investigation was to study the effect of TiB₂ addition on sintering behavior and mechanical properties of pressureless-sintered B₄C ceramic. Different amounts of TiB₂, mainly 5 t0 30 wt.% were added to the base material. Pressureless sintering was conducted at 2,050 and at 2,150 °C. Addition of 30 wt.% TiB₂ and sintering at 2,150 °C resulted in improving the density of the samples to about 99% of theoretical density. The composite samples exhibited very good mechanical properties (hardness, flexural strength and fracture toughness). As the amount of TiB₂ was increased further, the mechanical properties were reduced, except for the fracture toughness, apparently due to too much TiB₂ in the specimen.     

Microstructure and mechanical properties of pulsed electric current sintered B4C-TiB2 composites

Monolithic B₄C, TiB₂ and B₄C-TiB₂ particulate composites were consolidated without sintering additives by means of pulsed electric current sintering in vacuum. Sintering studies on B₄C-TiB₂ composites were carried out to reveal the influence of the pressure loading cycle during pulsed electrical current sintering (PECS) on the removal of oxide impurities, i.e. boron oxide and titanium oxide, hereby influencing the densification behavior as well as microstructure evolvement. The critical temperature to evaporate the boron oxide impurities was determined to be 2000 °C. Fully dense B₄C-TiB₂ composites were achieved by PECS for 4 min at 2000 °C when applying the maximum external pressure of 60 MPa after volatilization of the oxide impurities, whereas a relative density of 95-97% was obtained when applying the external pressure below 2000 °C. Microstructural analysis showed that B₄C and TiB₂ grain growth was substantially suppressed due to the pinning effect of the secondary phase and the rapid sintering cycle, resulting in micrometer sized and homogeneous microstructures. Excellent properties were obtained for the 60 vol% TiB₂ composite, combining a Vickers hardness of 29 GPa, a fracture toughness of 4.5 MPa m^1/2 and a flexural strength of 867 MPa, as well as electrical conductivity of 3.39E+6 S/m.     

Study on squeeze casting of an in situ 5 vol.-% TiB2/2014 Al composite

Abstract

An in situ 5 vol.-% TiB₂/2014 composite was prepared by an exothermic reaction of K₂TiF₆, KBF₄ and Al melts. The effect of introduction of in situ formed TiB₂ particles on the squeeze-casting formability of the composite was discussed. The microstructural evolution and changes in the mechanical properties of the composite at different squeeze pressures were investigated. The results showed that a pouring temperature of 710°C, a die temperature of 200°C and a squeeze pressure of 90 MPa were found to be sufficient to get the qualified squeeze cast and maximum mechanical properties for an Al 2014 alloy. However, the pouring temperature, die temperature and squeeze pressure need to be increased to 780°C, 250°C and 120 MPa for the composite to get the qualified squeeze cast and maximum mechanical properties as a result of the effect of introduction of in situ formed TiB₂ particles on the solidification process, plasticity and fluidity of the composite. The microstructural refinement, elimination of casting defects such as shrinkage porosities and gas porosities and improved distribution of TiB₂ particles in the case of the composite result when pressure was applied during solidification. Compared with the gravity-cast composite, the tensile strength, yield strength and elongation of the squeeze-cast composite at 120 MPa increased by 21%, 16% and 200%.     

Preparation and characterization of ZrB<Subscript>2</Subscript>-SiC ultra-high temperature ceramics by microwave sintering

ZrB₂-SiC ultra-high temperature ceramic composites reinforced by nano-SiC whiskers and SiC particles were prepared by microwave sintering at 1850°C. XRD and SEM techniques were used to characterize the sintered samples. It was found that microwave sintering can promote the densification of the composites at lower temperatures. The addition of SiC also improved the densification of ZrB₂-SiC composites and almost fully dense ZrB₂-SiC composites were obtained when the amount of SiC increased up to 30vol.%. Flexural strength and fracture toughness of the ZrB₂-SiC composites were also enhanced; the maximum strength and toughness reached 625 MPa and 7.18 MPa·m^1/2, respectively.     

Sintering and characterization of Al2O3-B4C composites

The effect of B₄C on the densification, microstructure and mechanical properties of pressureless sintered Al₂O₃-B₄C composites have been studied. Sintering was performed without sintering additives with varying B₄C content from 0–40 vol %. Up to 20 vol % B₄C, more than 97% theoretical density was always obtained when sintered at 1850 °C for 60 min. On increasing the sintering time from 30–120 min, there was no change in density. The result of X-ray diffraction analysis showed that no reaction occurred between Al₂O₃ and B₄C. The grain growth of Al₂O₃ was inhibited by B₄C particles pinned at the grain boundary and the grain-boundary drag effect. The critical amount of B₄C to drag the grain boundary migration effectively was believed to occur at 10 vol % B₄C sintered at 1850 °C for 60 min. The maximum three-point flexural strength was found to be 550 MPa for the specimen containing 20 vol % B₄C, and the maximum microhardness was 2100 kg mm^–2 for 30 vol % B₄C specimen.     

Preparation and characterization of ZrB2-SiC ultra-high temperature ceramics by microwave sintering

ZrB₂-SiC ultra-high temperature ceramic composites reinforced by nano-SiC whiskers and SiC particles were prepared by microwave sintering at 1850°C. XRD and SEM techniques were used to characterize the sintered samples. It was found that microwave sintering can promote the densification of the composites at lower temperatures. The addition of SiC also improved the densification of ZrB₂-SiC composites and almost fully dense ZrB₂-SiC composites were obtained when the amount of SiC increased up to 30vol.%. Flexural strength and fracture toughness of the ZrB₂-SiC composites were also enhanced; the maximum strength and toughness reached 625 MPa and 7.18 MPa·m^1/2, respectively.     

一种新的MoSi2基复合材料显微结构及其对力学性能的影响

本文研究了原位生成的ＴｉＣ／ＴｉＢ２／ＭｏＳｉ２三相复合材料的一种新的显微结构及其对力学性能的影响,结果表明,当热压金属Ｔｉ,Ｂ４Ｃ和ＭｏＳｉ２的混合粉末时,在ＭｏＳｉ２的基体内生成由ＴｉＣ和ＴｉＢ２组成的空心粒子。     

In situ reacted TiB2-reinforced alumina

In situ formation of TiB₂ in Al₂O₃ matrix through the reaction of TiO₂, boron and carbon has been studied. In hot-pressed samples, in addition to TiB₂, TiC and Al₂TiO₅ were also found to be dispersed phases in Al₂O₃ matrix. However, in the case of pressureless-sintered samples, pure Al₂O₃/TiB₂ composite with > 99% relative density can be obtained through a preheating step held at 1300°C for longer than 30 min and then sintering at a temperature above 1500°C. Pressureless-sintered composite containing 20vol% TiB₂ gives a flexural strength of 580 MPa and a fracture toughness of 7.2 MPa m^1/2.     

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.     

TiC-TiB2/Cu复合材料的自蔓延高温合成研究

采用SHS/PHIP工艺制备了TiC-TiB2/Cu复合材料,通过实验研究了该系列复合材料的微观结构特征和力学性能.结果表明,TiC-TiB2/Cu复合材料中只有TiC、TiB2和Cu相存在;随着Cu含量的增加,燃烧温度下降,材料的颗粒尺寸变小;TiC-TiB2/Cu复合材料的相对密度、抗弯强度和断裂韧性均随Cu含量的增加呈先增后减趋势,当Cu含量为20%时强度最高为580MPa,Cu含量为40%时韧性最高为8.1MPa.m1/2.     

Effect of Si additions on the microstructure and mechanical properties of hot-pressed B<Subscript>4</Subscript>C

Dense B₄C-based materials containing up to 4.9 wt % Si have been produced by hot pressing in the temperature range 1600–1700°C. In this process, the silicon melts to form a liquid phase, which improves the sinterability of the material. The boron carbide partially dissolves in the liquid Si to form silicon carbide between the B₄C grains. The relative density, bending strength, Vickers hardness, and fracture toughness of the materials obtained in this study are 99.0 ± 0.1%, 584 ± 12 MPa, 39.4 ± 0.1 GPa, and 5.3 ± 0.2 MPa m^1/2, respectively. The materials experience predominantly transcrystalline fracture.     

Properties of NbC-TiAl and TiB2-TiAI composites produced by plasma transferred arc process

Intermetallic compound based composites (IMCs) consisting of particles of NbC and TiB₂ in Ti-36 wt-%Al (NbC-TiAl and TiB₂-TiAl respectively), with varying volume fraction of reinforcing particles, were produced by a plasma transferred arc process. In NbC-TiAl IMCs, the hardness and 0·2% compressive proof stress increased steadily with increasing volume fraction of NbC whereas the tensile strength was lower than that of the unreinforced TiAl regardless of the volume fraction of NbC. In TiB₂-TiAl IMCs, the hardness and 0·2% compressive proof stress exhibited maximum values at a volume fraction of 5 vol.-%TiB₂. The maximum tensile strength of ～500 MN m^?2, which is almost twice that of the unreinforced TiAl, was obtained at a volume fraction of 5 vol.-%TiB₂. The initial improvement of mechanical properties due to the addition of TiB₂ was considered to be caused by the reinforcing effect of the TiB₂ particles, grain refinement, and the disappearance of γ grains in 3–5 vol.-%TiB₂-TiAl IMCs. The deterioration of the mechanical properties observed for a volume fraction of >5 vol.-%TiB₂ may be attributed to the increase in the amount of y grains with increasing volume fraction of TiB₂ particles from 7 to 15 vol.-% and the increase in coarse TiB₂ particles that can act as crack initiation sites in tensile tests.

MST/3434