Effect of graphite flake on the mechanical properties of hot pressed ZrB2-SiC ceramics

A ZrB₂ ceramic containing 20 vol.% SiC and 10 vol.% graphite flake (ZrB₂-SiC-G) was fabricated by hot pressing. It was shown that the fracture toughness was improved due to the introduction of graphite flake, whereas the flexure strength and hardness decreased slightly. The fracture toughness of ZrB₂-SiC-G composite was 6.1 ± 0.3 MPa·m^1/2, which was much higher than that of monolithic ZrB₂, ZrB₂-SiC composite and similar ZrB₂-SiC-C composite. The toughening mechanisms are crack deflection and branching as well as stress relaxation near the crack tip. The results here pointed to a potential method for improving fracture toughness of ZrB₂-based ceramics.     

Effect of annealing treatment on mechanical properties of a ZrB2-SiC-graphite ceramic

The ZrB₂-SiC-graphite (ZSG) ceramic was annealed at 1600, 1700 and 1800 °C for different times, respectively. It was revealed that the annealing treatment is favorable to increase the interface bonding and relative density, and to decrease the thermal residual stress, to result in the crimp of the graphite flake. It was the optimal annealing treatment process conditions of 1700 °C and 90 min according to the best combination of the mechanical properties. To compare the mechanical properties of the specimen before the annealing treatment, the hardness, strength and toughness of the specimen annealed at 1700 °C for 90 min were enhanced by 20.6% and 20.2%, decreased by 8.2%, respectively.     

Hot-pressed ZrB2–SiC–YSZ composites with various yttria content: Microstructure and mechanical properties

ZrB₂–10 vol%SiC–20 vol%YSZ composites were prepared by hot-pressed sintering with yttria content ranging from 2 mol% to 8 mol% in YSZ. The phase constitution, microstructure and mechanical properties of the composites were found to be strongly dependent on the yttria content. The average grain size became bigger for the composites with higher yttria content. When the yttria content was below 3 mol%, there is no cubic zirconia in the polished surface of composites, and the flexural strength of the composites was above 740 MPa. With the increase in yttria content, the fracture toughness fell down from 6.4 MPa m^1/2 to 5.6 MPa m^1/2. Vickers’ hardness of the hot-pressed composites varied above 18 GPa without obvious effect of the yttria content.     

Microstructure and mechanical properties of hot pressed ZrB2-SiCp-ZrO2 composites

The present paper investigated the microstructure and mechanical properties of ZrB₂-10 vol.%SiC_p-10 vol.%ZrO₂ composites hot pressed at three temperatures. Phase transformability from t-ZrO₂ to m-ZrO₂ during fracture was analyzed through calculating the volume fractions of m-ZrO₂ and t-ZrO₂ on polished and fracture surfaces. The densification temperature was found to have a significant effect on the microstructure, phase transformation and the properties of the composites. When the composite was hot pressed at 1950 °C, the average grain size was 9.5 µm, and the fracture toughness was 4.5 MPa·m^1/2. Comparatively, when the composite was hot pressed at 1750 °C, the average grain size was 3.4 µm, and the fracture toughness increased by ~ 50% to 6.8 MPa·m^1/2.     

A technique for ultrahigh temperature oxidation studies of ZrB2-SiC

A new oxidation method, high frequency induction heating, was introduced to investigate the rapid oxidation characteristics of ZrB₂-SiC at 1800 °C up to 50 min. A high temperature was achieved within 30 s by adjusting the current or voltage. According to the isothermal test at 1800 °C, the oxidation kinetics for the composite followed a para-linear law. The specific weight gains increased from 4.86 to 12.89 mg/cm² when the exposure time increased from 10 to 50 min. When exposure for 30 min, a thin outmost layer of SiO₂, a ZrO₂ layer and a thick SiC-depleted layer formed on the surface of specimens. The structural characteristic of oxidation layer obtained by high frequency induction heating was similar to those formed by standard oxidation furnace.     

Effect of Nb2O5 on the microstructure and mechanical properties of TiAl based composites produced by hot pressing

In situ composites of TiAl reinforced with Al₂O₃ particles are successfully synthesized from an elemental powder mixture of Ti, Al and Nb₂O₅ by the hot-press-assisted reaction synthesis (HPRS) method. The as-prepared composites are mainly composed of TiAl, Al₂O₃, NbAl₃, as well as small amounts of the Ti₃Al phase. The in situ formed fine Al₂O₃ particles tend to disperse on the matrix grain boundaries of TiAl resulting in an excellent combination of matrix grain refinement and uniform Al₂O₃ distribution in the composites. The Rockwell hardness and densities of TiAl based composites increase gradually with increasing Nb₂O₅ content, and the flexural strength and fracture toughness of the composites have the maximum values of 634 MPa and 9.78 MPa m^1/2, respectively, when the Nb₂O₅ content reaches 6.62 wt.%. The strengthening mechanism was also discussed.     

弱界面层方向性对层状ZrB2-SiC/石墨陶瓷的影响

利用流延-叠层-热压烧结工艺制备层状ZrB_2-SiC/石墨(ZrB_2-SiC/G)陶瓷,研究了石墨弱界面层的方向性对其力学性能的影响;通过XRD、SEM等对层状ZrB_2-SiC/G陶瓷的物相、形貌进行观察分析。结果表明:层状ZrB_2-SiC/G陶瓷在平行方向上的弯曲强度为(382±25)MPa,略低于垂直方向的弯曲强度((429±30)MPa);平行方向的断裂韧性为(11.2±0.3)MPa·m~(1/2),比垂直方向的断裂韧性提高了75%。层状ZrB_2-SiC/G陶瓷在平行方向上的断裂韧性的提高主要是由于石墨弱界面层对裂纹的偏转、分叉和脱层作用。     

高温氧化及热震对SiC/ZrB2-SiC/SiC涂层炭/炭复合材料力学行为的影响

为提高炭/炭(C/C)复合材料的高温抗氧化性能,同时分析涂层制备及高温氧化对涂层材料力学行为的影响,在C/C复合材料表面采用反应熔渗、料浆涂刷结合化学气相沉积工艺制备了SiC/ZrB2-SiC/SiC三层高温抗氧化涂层。利用SEM和XRD分析复合涂层的微观结构和相组成,考察涂层复合材料1500℃高温抗氧化和1500℃-室温的抗热震性能,研究高温氧化及热震对涂层C/C复合材料力学行为的影响。结果表明,复合涂层试样1500℃静态空气环境下具有优异的抗氧化及抗热震性能:1500℃氧化20 h后试样保持增重,1500℃至室温热震50次后增重为0.69%。因涂层制备过程中粉料的渗入反应,复合材料弯曲强度增长了7.08%。在经历1500℃氧化20 h和1500℃至室温50次热震后,涂层复合材料弯曲强度有所下降,且因材料界面结合力的减弱使得纤维拔出特征明显,材料塑性断裂特征增强。     

烧结温度对反应热压烧结制备ZrB2-ZrC-W2Zr复合材料组织和力学性能的影响

以B_4C、Zr、W为原料,采用反应热压烧结工艺制备了ZrB_2-ZrC-W_2Zr复合材料,系统研究了烧结温度对复合材料组织结构和力学性能的影响规律。结果表明,复合材料主要由ZrB_2、ZrC、W_2Zr和少量的W组成,随着烧结温度从1 600℃升高到1 900℃,W的含量略有增加,W_2Zr的含量略有减少,ZrB_2晶粒的形态由针状向板条状转变,晶粒尺寸逐渐增大,而长径比逐渐减小。复合材料的抗弯强度和断裂韧性随着烧结温度的升高先增大后减小,在1 850℃出现峰值,分别达到约560 MPa和5.5 MPa·m~(1/2)。     

Preparation and properties of 2D C/ZrB2-SiC ultra high temperature ceramic composites

Two-dimensional C/ZrB₂-SiC composites were fabricated by chemical vapor infiltration (CVI) process combined with slurry paste (SP) method. ZrB₂ was introduced in the matrix by stacking the pasted carbon cloth with ZrB₂-polycarbosilane slurry. After heat-treated at 900 °C, the stacked carbon cloth preform was infiltrated SiC by CVI process to obtain 2D C/ZrB₂-SiC composites. Mechanical properties such as flexural strength and interlaminar shear strength were investigated. The ablation tests were carried out on an oxyacetylene torch flame. The small linear erosion rates indicate that the composites have good ablation resistance properties. These results demonstrate that CVI combined with SP method is a useful way to fabricate 2D C/ZrB₂-SiC composites.     

C/C复合材料ZrB2基超高温陶瓷涂层的研究进展

ZrB₂基超高温陶瓷因其优异的高温抗氧化和烧蚀等性能,成为C/C复合材料理想的热防护涂层材料。本文从以下几个方面对C/C复合材料表面用ZrB₂基超高温陶瓷涂层的研究现状进行了综述:介绍了ZrB₂基超高温陶瓷涂层体系的主要制备技术,并对比了其制备的涂层抗氧化性和抗烧蚀性,总结了各制备方法的优点与不足;从单元、双元、三元材料掺杂改性的角度,详述了ZrB₂基复合涂层常见的材料体系,总结了其改性思路;介绍了ZrB₂基涂层在多层结构设计与开发方面的研究现状。最后简要展望了ZrB₂基超高温陶瓷涂层未来的研究方向。     

Mechanical properties and microstructure of Al2O3/TiAl in situ composites doped with Cr2O3

Al₂O₃/TiAl composites were successfully fabricated from powder mixtures of Ti, Al, TiO₂ and Cr₂O₃ by a hot-press-assisted exothermic dispersion method. The effect of the Cr₂O₃ addition on the microstructures and mechanical properties of Al₂O₃/TiAl composites was characterized, and the results showed that the Rockwell hardness, flexural strength and fracture toughness of the composites increased as the Cr₂O₃ content increased. When the Cr₂O₃ content was 2.5 wt%, the flexural strength and the fracture toughness attained peak values of 925 MPa and 8.55 MPa m^1/2, respectively. This improvement of mechanical properties was due to the more homogeneous and finer microstructure developed from the addition of Cr₂O₃ and an increase in the ratio of α₂-Ti₃Al to γ-TiAl matrix phases.     

Modulation periods and ratios induced changes of microstructure and mechanical properties of AlN/ZrB2 multilayered coatings

AlN/ZrB₂ multilayered coatings were synthesized in a magnetron sputtering system. The extensive measurements were employed to investigate the influence of different nanoscale modulation periods and modulation ratios on microstructure and mechanical properties of the coatings. Analysis of X-ray diffraction, profiler and nanoindention indicated that multilayered coatings possessed much higher hardness and elastic modulus than monolithic AlN and ZrB₂ coatings. At the substrate negative bias of −80 V, maximum hardness (34.1 GPa) and elastic modulus (469.8 GPa) were obtained in the multilayer with Λ = 30 nm and t_AlN:t_ZrB2 = 1:3. This hardest multilayer showed a marked polycrystalline structure with the strong mixture of ZrB₂ (001), ZrB₂ (100), ZrB₂ (101), AlN (100) textures.     

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.     

Influence of in situ formed ZrB2 particles on microstructure and mechanical properties of AA6061 metal matrix composites

Particulate reinforced metal matrix composites (PMMCs) have gained considerable amount of research emphasis and attention in the present era. Research is being carried out across the globe to produce new combination of PMMCs. PMMCs are prepared by adding a variety of ceramic particles with monolithic alloys using several techniques. An attempt has been made to produce aluminium metal matrix composites reinforced with zirconium boride (ZrB₂) particles by the in situ reaction of K₂ZrF₆ and KBF₄ salts with molten aluminium. The influence of in situ formed ZrB₂ particles on the microstructure and mechanical properties of AA6061 alloy was studied in this work. The in situ formed ZrB₂ particles significantly refined the microstructure and enhanced the mechanical properties of AA6061 alloy. The weight percentage of ZrB₂ was varied from 0 to 10 in steps of 2.5. Improvement of hardness, ultimate tensile strength and wear resistance of AA6061 alloy was observed with the increase in ZrB₂ content.     

Microstructure and mechanical properties of TiAlN/SiO2 nanomultilayers synthesized by reactive magnetron sputtering

TiAlN/SiO₂ nanomultilayers with different SiO₂ layer thickness were synthesized by reactive magnetron sputtering. The microstructure and mechanical properties were investigated by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and nano-indentation. The results indicated that, under the template effect of B1-NaCl structural TiAlN layers, amorphous SiO₂ was forced to crystallize and grew epitaxially with TiAlN layers when SiO₂ layer thickness was below 0.6 nm, resulting in the enhancement of hardness and elastic modulus. The maximum hardness and elastic modulus could respectively reach 37 GPa and 393 GPa when SiO₂ layer thickness was 0.6 nm. As SiO₂ layer thickness further increased, SiO₂ transformed back into amorphous state and broken the coherent growth of nanomultilayers, leading to the decrease of hardness and elastic modulus.     

Microstructure and high-temperature strength of textured and non-textured ZrB2 ceramics

Zirconium diboride (ZrB₂) ceramic possesses a unique combination of nice mechanical performance, high melting point (> 3000 °C) and great high-temperature oxidation resistance (up to 1600 °C), which makes it a promising material system for ever-increasing ultra-high temperature (UHT) applications. However, ZrB₂ suffers from poor mechanical performance at UHTs, which could strongly limit its applications at UHT. Here, we successfully demonstrate that texturing is an effective strategy to greatly enhance the flexural strength of monolithic ZrB₂, reaching a high value of 810 ± 60 MPa at 1600 °C when loaded in c-axis direction. We thoroughly discuss the strengthening mechanism by in-depth microstructural observations and analysis. Our discovery has technological and scientific implications for other UHT ceramic systems, especially those using ZrB₂ as a matrix.     

First principles investigation on the structural, mechanical and electronic properties of OsC2

The structural, mechanical and electronic properties of OsC₂ were investigated by use of the density functional theory. Seven structures were considered, i.e., orthorhombic Cmca (No. 12, OsSi₂), Pmmn (No. 59, OsB₂) and Pnnm (No. 58, OsN₂); tetragonal P4₂/mnm (No. 136, OsO₂) and I4/mmm (No. 139, CaC₂); cubic Fm–3m (No. 225, CaF₂) and Pa-3 (No. 205, PtN₂). The results indicate that Cmca in OsSi₂ type structure is energetically the most stable phase among the considered structures. It is also stable mechanically. OsC₂ in Pmmn phase has the largest bulk modulus 319 GPa and shear modulus 194 GPa. The elastic anisotropy is discussed.     

Influence of CaTiO3 impurity in SHS-TiN powder on the mechanical properties of ZrO2–TiN composites

Yttria-stabilised tetragonal polycrystalline ZrO₂-based composites with 40 vol.% TiN were hot pressed at 1450 °C for 1 h using a jet-milled thermally synthesized and a self-propagating high-temperature synthesis (SHS) TiN powder. The ZrO₂ phase of the SHS-TiN powder-based composites was found to be substantially coarser than for the jet-milled TiN powder-based ceramics and prone to spontaneous transformation to m-ZrO₂ and microcracking, due to the CaTiO₃ impurity in the SHS-TiN starting powder. In order to prove this, a set of experiments was performed to investigate the effect of the addition of CaO and TiO₂ on an yttria-stabilised tetragonal ZrO₂ polycrystalline (Y-TZP). The addition of 0.2 mol% of CaO to a Y-TZP ceramic was found to destabilise the t-ZrO₂ phase, whereas the addition of 1 mol% TiO₂ results in significant grain growth and the formation of less transformable t-ZrO₂. The CaTiO₃ impurity could be removed from the SHS-TiN powder by hot hydrochloric acid leaching, allowing to obtain a similar microstructure and mechanical properties as with conventional TiN powder.     

熔盐对ZrO2纤维模板辅助燃烧合成ZrB2纤维的影响

以ZrO₂纤维、B₂O₃粉、Mg粉为原料,分别以NaCl、MgCl₂及NaCl、MgCl₂复合盐为稀释剂,采用模板辅助燃烧合成法,经酸洗制备了ZrB₂短纤维,采用试算法计算了反应体系绝热温度,并对产物进行XRD和SEM表征。结果表明:反应体系的绝热温度随着熔盐掺量的增加而降低,掺NaCl体系绝热温度下降较为明显,尤其是在熔盐掺量较高的情况下。加入NaCl后产物物相主要为ZrB₂以及少量残余的ZrO₂,加入MgCl₂后产物中还有少量Mg₃B₂O₆。加入熔盐不仅能避免ZrO₂纤维的熔融,使产物更容易保持原料中纤维的形状,还能减小产物的晶粒尺寸,加入MgCl₂能促进产物晶粒的发育,随着MgCl₂掺量的增加,纤维上的颗粒逐渐发育成棱角分明的六方状晶体。从残余的ZrO₂含量和晶粒尺寸分析,单盐的效果要优于复合盐,MgCl₂的效果优于NaCl。