Structural evaluation and mechanical property of boron nitride fibers during melt‐drawn fabrication process

Boron nitride (BN) fibers were fabricated on a large scale through the melt‐drawn technique from low‐cost boric acid, NH₃, and N₂. Evolution of structure and properties of BN fibers during the fabrication process was studied by Fourier transform infrared (FT‐IR), X‐ray diffraction (XRD), scanning electron microscope (SEM), and X‐ray photoelectron spectroscopy (XPS). The mechanical properties of BN fibers were tested and analyzed. The results shown that both the mechanical properties and the crystallinity of BN fibers slightly increased with the temperature from 450 to 850°C, due to the combination of the fused‐B₃N₃. For BN fibers heat‐treated at 850 or 1000°C, the tensile strength (σ^R) and elastic modulus (E) were strongly increased because of the increase in crystallization of the BN phase. The meso‐hexagonal BN fibers with a diameter of 5.0 μm were fabricated at 1750°C, of which the tensile strength (σ^R) and elastic modulus (E) are 1200 MPa and 85 GPa, respectively. BN fibers with excellent mechanical properties and proper diameters were obtained by nitriding of green fibers during their conversion into ceramic.     

Synthesis and microwave dielectric properties of new high quality Mg2NdNbO6 ceramics

New high‐quality microwave dielectric ceramics Mg₂NdNbO₆ were prepared by conventional solid‐state sintering method. The phases, micro‐structures and microwave dielectric properties of Mg₂NdNbO₆ ceramics were investigated at sintering temperature in the range of 1275°C‐1400°C. The X‐ray diffraction patterns showed that the peaks of the compounds were attributed to two phases, including the main crystalline phase of NdNbO₄ that was indexed as the monoclinic phase and MgO as the second phase. Well‐developed microstructures of Mg₂NdNbO₆ ceramics can be achieved, and the grain size reached the maximum value (1.63 μm) at 1375°C. As the sintering temperature increased, the dielectric constant, temperature coefficient of resonant frequency and apparent density remained almost unchanged, however, the significant change in the quality factor was observed. At 1375°C, Mg₂NdNbO₆ ceramics possessed excellent microwave dielectric properties: ε_r = 16.22, Q × f = 116 000 GHz and τ_f = ?30.96 ppm/°C.     

Degradation of Nextel™ 610‐based oxide‐oxide ceramic composites by aluminum oxychloride decomposition products

Nextel? 610 alumina fibers and alumina‐YAG (yttrium‐aluminum garnet) matrices were used to make oxide‐oxide ceramic matrix composites (CMCs) with and without monazite (LaPO₄) fiber‐matrix interfaces. Twelve sequential aluminum oxychloride (AlOCl) infiltrations with 1 hour heat treatments at 1100°C and a final 1 hour heat treatment at 1200°C were used for matrix densification. This matrix processing sequence severely degraded CMC mechanical properties. CMC tensile strengths and interlaminar tensile (ILT) strengths were less than 10 MPa and 1 MPa, respectively. Axial fracture of Nextel? 610 fibers was observed after ILT testing, highlighting the extreme degradation of fiber strength. Extensive characterization was done to attempt to determine the responsible degradation mechanisms. Changes in Nextel? 610 fiber microstructure after CMC processing were characterized by optical microscopy, SEM, and extensively by TEM. In AlOCl degraded fibers, grain boundaries near the fiber surface were wetted with a glass that contained Y₂O₃/SiO₂ or Y₂O₃/La₂O₃/P₂O₅/SiO₂, and near‐surface pores were partially filled with Al₂O₃. This glass must also contain some Al₂O₃ and initially some chlorine. AlOCl decomposition products were predicted using the FactSage^® Thermochemical code, and were characterized by mass spectrometry. Effects of AlOCl precursors on monazite coated and uncoated Nextel? 610 fibers tow and filament strength were evaluated. A mechanism for the severe degradation of the oxide‐oxide CMCs and Nextel? 610 fibers that involves subcritical crack growth promoted by release of chlorine containing species during breakdown of intergranular glasses in an anhydrous environment is proposed.     

Growth of diopside crystals in CMAS glass‐ceramics using Cr2O3 as a nucleating agent

CaO–Al₂O₃–MgO–SiO₂ (CAMS)‐based glass‐ceramics were prepared using body crystallization method. Adding Cr₂O₃ into the ceramics not only effectively lowered the crystallization temperature, but also led to significant grain refinement of diopside that crystallized in the CAMS glass‐ceramic after crystallization treatment at 900°C for 2 hours. Experimental work verified that the epitaxial growth of the diopside on the spinel particles, which formed during nucleation treatment when fabricating the glass‐ceramics, facilitated the heterogeneous nucleation of diopside on the spinel and refined the diopside. In addition, two energetically favored crystallographic orientation relationships between the epitaxial growth diopside and spinel were experimentally observed. They are //[001]_diopside,////(200)_diopside and //[101]_diopside, (311)_spinel//. These two novel results can be potentially used to develop new glass‐ceramic materials with improved performance.     

Assessment of conversion efficiency of Cr4+ ions by aliovalent cation additives in Cr:YAG ceramic for edge cladding

0.25at.% Cr:YAG ceramics were successfully fabricated as the edge cladding of Yb:YAG transparent ceramic slabs through vacuum sintering of co‐precipitated powders, using oxide additives to introduce different cations. The effects of various cation additives (Si⁴⁺, Ca²⁺, and Si⁴⁺ + Ca²⁺) on the conversion efficiency of Cr⁴⁺ ions and optical characteristics of the Cr:YAG edge cladding were investigated. Measurements of the absorption spectra of the Cr:YAG ceramics without any additives revealed 2 absorption bands centered at 430 nm and 600 nm, which imparted the sample with a green color. The introduction of only Si⁴⁺‐bearing additive did not promote the transition of Cr ions from the 3+ to 4+ state. Theoretical analysis and experimentation revealed that the addition of CaO not only enhanced the microstructure and improved the transmittance of the Cr:YAG ceramic, but also introduced vacancies that assisted in the formation of Cr⁴⁺ ions. It was determined that CaO has the same effect on the conversion efficiency of Cr⁴⁺ ions whether it is added as a single additive or in combination with SiO₂. The underlying mechanisms by which these aliovalent cation additives influence the formation of Cr⁴⁺ ions and affect optical properties are discussed in detail. High quality composite ceramics with Yb:YAG transparent ceramic slabs and dark brown‐colored Cr⁴⁺: YAG ceramic edge cladding were achieved through the addition of 0.05 wt.% CaO to the edge cladding, with no interfacial effects between the 2 regions being observed.     

Effect of additive structure and size on SiO2 formation in polymer‐derived SiOC ceramics

Silicon oxycarbide (SiOC) ceramics with highly adjustable properties and microstructures have many promising applications in batteries, catalysis, gas separation, and supercapacitors. In this study, additive structures on the nucleation and growth of SiO₂ within SiOC ceramics are investigated by adding cyclic tetramethyl‐tetravinylcyclotetrasiloxane (TMTVS) or caged octavinyl‐polyhedral oligomeric silsesquioxane (POSS) to a base polysiloxane (PSO) precursor. The effects of the 2 additives on the polymer‐to‐ceramic transformation and the phase formation within the SiOC are discussed. POSS encourages SiO₂ nucleation and leads to more SiO₂ formation with significantly increased ceramic yield, which subsequently leads to higher specific surface of 1557 m²/g with a larger pore size of ～1.8 nm for the porous SiOC. High TMTVS content decreases both the specific surface area and pore volume of the resulting porous SiOCs. This study demonstrates a new approach of using Si‐rich additive POSS to increase the SiOC yield while maintaining or even increasing the specific surface area.     

SiC晶须,晶板增韧AlN陶瓷的研究

本文利用现代测试技术对ＳｉＣｗ,ＳｉＣｐ增韧ＡｌＮ材料的力学性能,显微结构进行研究,并分析探讨了材料的增韧机理,结果表明;ＳｉＣｗ可有效改善材料的断裂韧性和断裂强度,其增韧机理主要为裂纹偏转和晶须拔出效应,ＳｉＣｐ加入的断裂韧性起到良好的促进作用,但对材料的断裂强度则有不良的作用,其增韧机理主要为裂纹偏转和分枝效应。     

相变增韧和层状复合协同强韧化Al2O3陶瓷

本文采用相变增韧和层状复合协同强韧化Ａｌ２Ｏ３复合陶瓷,相变增韧制备出ＺＴＡ陶瓷,在此基础上,采用层状复合工艺,制备出ＺＴＡ／ＢＮ陶瓷。研究结果表明：相变增韧和层状复合协同强韧化Ａｌ２Ｏ３能基本保持陶瓷抗弯强度,冲击韧性提高了３７倍。     

Thermal evolution and crystallisation of polydimethylsiloxane–zirconia nanocomposites prepared by the sol–gel method

Polydimethylsiloxane–zirconia nanocomposites have been prepared by hydrolysis of diethoxydimethylsilane and zirconium n-propoxide in different molar ratios. Transparent, homogeneous and non-porous xerogels have been obtained up to 70 mol% ZrO₂ content. The starting xerogels have been pyrolyzed under argon atmosphere up to 1400°C and the structural evolution of samples treated at different temperatures has been followed by X-ray diffraction, transmission electron microscopy, infrared and ²⁹Si solid state nuclear magnetic resonance spectroscopies, thermal analyses and N₂ sorption measurements. The polymer-to-ceramic conversion leads to the structural rearrangement of the siloxane component with the production at 600°C of high surface area materials with pore sizes below 3 nm. Samples are amorphous up to 800°C. At 1000°C, the structural evolution of the silicon moiety produces an amorphous oxycarbide phase whereas the primary crystallisation of tetragonal zirconia takes place, with crystallinity and crystallite sizes depending on the ZrO₂ content. At 1400°C, the silicon oxycarbide phase generates a mixture of amorphous silica and crystalline silicon carbide polymorphs. In this matrix, tetragonal and monoclinic ZrO₂ phases are present with ZrO₂ average crystallite dimensions never exceeding 20 nm, for ZrO₂ content ≤50 mol%. The tetragonal/monoclinic ratio as well as the crystallite sizes appear strictly related to the chemical composition. ©     

纳米碳颗粒/碳化硅陶瓷基复合材料的氧化行为

以微米硅(Si)和纳米碳黑(Cp)粉体为主要原料,采用经机械化学法合成的碳化硅(SiC)和15%和25%的纳米碳颗粒与碳化硅(Cp-SiC)的复合粉体,并经无压烧结得到了Cp/SiC陶瓷基复合材料,分析了在不同温度条件下Cp/SiC烧结体的氧化行为。结果表明:当温度小于700℃时,Cp/SiC复合陶瓷在空气中的氧化受C—O2反应控制,致使其为均匀氧化;700℃时,氧化后的复合材料显气孔率最大,弯曲强度达极小值;大于700℃,氧化过程受O2的气相扩散控制,呈非均匀氧化;700~900℃之间,O2通过微裂纹的扩散控制着Cp/SiC的氧化过程;900~1 100℃之间,O2通过SiC缺陷的扩散控制着Cp/SiC的氧化过程,并在1 000℃时的最初的2 h内,复合材料弯曲强度增大,且达到了极大值。同时表明,纳米碳含量是影响复合材料强度及氧化行为的关键因素,添加纳米碳质量分数为15%的Cp/SiC复合陶瓷可以作为一种抗氧化性能优良的玻璃夹具材料。