高固体分含氟羟基丙烯酸酯树脂的合成及性能研究

分别以甲基丙烯酸十二氟庚酯、甲基丙烯酸六氟丁酯为含氟单体,采用硫代甘油为链转移剂,通过自由基溶液聚合制备了2种含氟羟基丙烯酸酯树脂,考察了硫代甘油用量对树脂相对分子质量、黏度及羟基含量的影响,对树脂结构和热稳定性进行了表征;同时以多异氰酸酯为固化剂制备了聚氨酯涂膜,并对涂膜的表面能、光学透过性、耐化学品性以及常规物理性能进行了测试。结果表明:在硫代甘油用量为4%、固体分含量为60%的条件下,2种树脂的相对分子质量和黏度分别低至1 891、(231±2)mPa·s和2 144、(362±3)mPa·s;聚氨酯涂膜具有一定的疏水性,在可见光区范围内,涂膜光透过率大于98%,并具有良好的耐化学品性及常规物理性能。     

Effect of temperature on the growth of boron nitride interfacial coatings on SiC fibers by chemical vapor infiltration

In order to improve bonding property between SiC fibers and matrix of SiC_f/SiC composites, boron nitride (BN) interfacial coatings were synthesized by chemical vapor infiltration. BN coatings were fabricated from BCl₃–NH₃ gaseous mixtures at four different temperatures (843 °C, 900 °C, 950 °C and 1050 °C) with different deposition times. Growth kinetics, nucleation and growth processes, microstructure and chemical composition of boron nitride coatings were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Raman spectrometry. Results showed that deposition rate increased as the temperature increased from 843 °C to 950 °C. However, deposition rate decreased slightly from 23.10 ± 0.85 nm/min (950 °C) to 21.39 ± 0.67 nm/min when the temperature was increased further to 1050 °C. It could be due to the nucleation occurring in the gas and the consumption of a large amount of BCl₃ and NH₃. When deposition temperature was 843 °C, BN grains deposited on top layer of the coating could not completely cross Ehrlich-Schwoebel barrier and grew in island growth mode. On the other hand, the deposition pattern followed a layer-by-layer growth mode when deposition temperature was 1050 °C. Deposition temperature significantly affected the microstructure of as-deposited BN coatings. At 843 °C, 950 °C and 1050 °C, the coatings presented amorphous, polycrystalline and hexagonal structures, respectively.     

Deposition and characterization of hex-BN coating on carbon fibres using tris(dimethylamino)borane precursor

Boron nitride thin films were deposited on carbon fibres by chemical vapor deposition from the single source precursor tris(dimethylamino)borane (TDMAB). Hydrogen was used as carrier gas and additional nitrogen was supplied in the form of ammonia. The heating of the substrate was performed by Joule effect. Detailed TEM structural and chemical analyses reveal a meso-graphitic structure with a stoichiometric B/N ratio as confirmed by Auger Electron Spectroscopy (AES). A penetration of carbon element from the fibre was observed in the BN layer close to the interface.     

Effect of multi-component rare-earth doping on maintaining structure stability of RE2Zr2O7 (RE = La,Sm, Gd,Y, Yb) coatings under thermal cycling

Inspired by the high entropy effects of high-entropy components, a novel high-entropy rare-earth zirconate (La_1/5Gd_1/5Y_1/5Sm_1/5Yb_1/5)₂Zr₂O₇ (HEC-LZ) was designed and successfully synthesized in this work. In addition, two binary rare-earth doped zirconates (RE-LZ), (La_1/3Sm_1/3Yb_1/3)₂Zr₂O₇ (LSYZ) and (La_1/3Gd_1/3Y_1/3)₂Zr₂O₇ (LGYZ), were proposed using the same rare-earth elements for comparison. The thermal barrier coatings with LZ-based ceramic top layer were prepared by spray granulation, solid-phase synthesis and atmospheric plasma spraying techniques. The as-synthesized LZ-based ceramics are all dominated by the pyrochlore phase. Under 1000 °C, the thermal cycling performances of the three coatings were studied. The microstructure evolution and crack expansion during the failure process were investigated in detail. The strengthening mechanism and the cause of coating spallation are proposed in combination with mechanical properties and thermal matching analysis. The results showed that compared with the undoped LZ coating, the thermal shock life of LGYZ coating, LSYZ coating and HEC-LZ coating is improved by nearly 46%, 27% and 57%, respectively. Due to the characteristics of high randomness, HEC-LZ ceramic has a large lattice distortion than RE-LZ ceramics, resulting in a higher coefficient of thermal expansion and fracture toughness, which contributes to maintaining the structure stability of coatings under thermal stress.     

Oxidation behavior of 3D Hi-Nicalon/SiC composite exposed in wet and simulated air environments

Oxidation behavior of a 3D Hi-Nicalon/SiC composite was investigated in wet and simulated air with a flow rate of 3.5 cm s⁻¹ at temperatures above 1000 °C. Results showed that oxidation was occurred mainly on the specimens surface and rate-controlled by oxygen diffusion for both oxidation environments. Silica formed in wet air was viscous and thicker. After oxidation, strength deterioration of the composite was associated mainly with the degradation of Hi-Nicalon fiber. Meanwhile, the difference in fracture behavior could be attributed to the change of fiber/matrix interface bonding caused by high temperature oxidation.     

7050-T7451铝合金阳极氧化膜在模拟舰载环境下的腐蚀行为及疲劳性能衰减研究

通过酸性盐雾试验研究了经苹果酸?硫酸体系阳极氧化处理的7050-T7451铝合金在模拟舰载环境中的腐蚀行为。通过扫描电子显微镜、电化学阻抗谱测量和疲劳性能测试分析了经酸性盐雾腐蚀不同时间后阳极氧化膜结构和基体疲劳寿命的变化。结果表明,阳极氧化膜对铝合金基体具有很好的保护作用,能够保护铝合金基体在酸性盐雾试验的4个周期(192 h)内免受腐蚀。随着酸性盐雾试验时间的延长,阳极氧化7050-T7451铝合金的疲劳寿命逐渐衰减,其演化规律与腐蚀行为的变化基本吻合。     

Fatigue strength and fracture mechanism of steel modified by super-rapid induction heating and quenching

Four kinds of surface hardened-specimens (ordinary structural steel with carbon content of 0.45% C) having hardened thicknesses of 0.7–1.8 mm were prepared using a ‘super-rapid induction heating (SRIH) system’. Rotation bending fatigue tests were performed with special focus on the effect of a hardened thickness on fatigue properties. Measurement of residual stress and observation of the fracture surface were also carried out to investigate the fracture mechanism of the specimen with a shallow hardened layer. It was found that there is not much improvement of fatigue strength at 10⁷ cycles for specimens with shallow hardened layers in spite of having a high compressive residual stress of about 1000 MPa. This is because the fatigue crack originating from inside the hardened layer leads to the final fracture of the specimen (internal fracture mode). Improvement of fatigue strength has been achieved on the specimen with thick hardened layers, such as those about 1.8 mm thick. In this case, fatigue cracks originate from inclusions located in hardened layers, which leads to final fracture (hardened-layer fracture mode).     

Microstructure and mechanical performance of SiCf/BN/SiC mini-composites oxidized at elevated temperature from ambient temperature to 1500 °C in air

SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapour deposited (CVD) BN interface layers were fabricated. The mechanical performance and binding strength of the composites and the fibre/interface for the oxidized SiC_f/BN/SiC mini-composite samples (oxidation at 1000, 1200, 1300, 1400 and 1500 °C in air for two hours) were investigated by tensile tests and fibre push-out tests, respectively. The value of oxidation mass change was also measured. Some unusual phenomena for the SiC_f/BN/SiC mini-composites oxidized at 1000 °C were discovered in this work. The tensile strength reached a maximum value, and the mass gain rate showed as a singular negative value, while the shear strength between the fibre and the matrix was moderate. Scanning electron microscopy, energy dispersive spectrometry, infrared spectroscopy and X-ray diffraction characterization methods were used to reveal the microstructural evolution and investigate the unusual phenomenon during oxidation procedures. This work will provide guidance for predicting the service life of SiC_f/BN/SiC composite materials and may enable these materials to become a backbone for thermal structure systems in aerospace applications.     

Thermal cycling behavior of plasma-sprayed yttria-stabilized zirconia thermal barrier coating with La0.8Ba0.2TiO3−δ top layer

In this study, a La_0.8Ba_0.2TiO_3?δ (LBT) upper layer was deposited on an yttria-stabilized zirconia (YSZ) thermal barrier coating (TBC) through atmospheric plasma spraying. The thermal cycling behaviors of the YSZ single-ceramic-layer and LBT–YSZ double-ceramic-layer coatings at 1000 °C were investigated through a water quenching method. Moreover, phases, microstructural evolution, and elemental distributions were studied through by X-ray diffraction and scanning electron microscopy–energy-dispersive X-ray spectroscopy. The results showed that the thermal cycling lifetime of the LBT–YSZ coating was 27% higher than that of conventional YSZ coating. The conventional YSZ coating failed after 251 cycles because of the joining of the continuous horizontal and vertical cracks caused by the formation of thermal growth oxides and the bending effect of the single-ceramic-layer structure. The thermal cycling behavior of the LBT–YSZ coating was different from that of the YSZ coating at the edge and center. Although the former was similar to the failure behavior of the YSZ coating, the cracks in the vertical direction were deflected as a result of the bending effect of the double-ceramic-layer structure during quenching. This deflection led to the formation of slope cracks with longer propagation paths and slope spallation zones. The latter showed small-debris spallation on top of the LBT upper layer due to the lower fracture toughness of the LBT, which protected the central coating from the structural damage of the ceramic coating. These two behaviors would either release the thermal stress or increase the crack-propagation energy requirement in the ceramic coating, consequently improving the thermal cycling lifetime of the LBT–YSZ coating. In summary, depositing an LBT upper layer could potentially improve the thermal cycling lifetimes of TBCs.     

Structure,dielectric, and ferroelectric properties of (1-x)Bi0.5Na0.5TiO3 – X K0.5Na0.5NbO3 (0 ≤ x ≤ 0.1) solid solution

The correlation of the phase structure, dielectric, and ferroelectric properties of lead-free (1-x)(Na_0.5Bi_0.5)TiO₃–xK_0.5Na_0.5NbO₃ (NBTKNx) (0 = x ≤ 0.1) polycrystalline ceramics, fabricated via a solid state reaction technique, were investigated. The Rietveld refinement allowed identifying the crystallographic transformation from a rhombohedral to a coexisting rhombohedral-tetragonal or tetragonal long range-ordered ferroelectric (FE) phase. The dielectric investigations showed an increase of the dielectric diffuseness (1.53 = γ ≤ 1.73) and a clear shift of the depolarization temperature (T_d) to a lower temperature while increasing substitution. More importantly, the lattice disorder also generated a plateau-like dielectric anomaly, leading to a thermally stable ϵ_r ∼2859 ± 20% (120–500 °C) and ∼3112 ± 10% (120–420 °C) for x = 0.075 and 0.1 samples, respectively. At room temperature (RT), Raman spectroscopy investigations revealed a downshift of the frequencies as a function of the composition with an inhomogeneous broadening of the Raman lines. On heating, Raman spectra showed changes in the region where the dielectric transitions are observed. Moreover, the composition dependence of the current peaks in the I-E loops confirmed the occurrence of a phase transition from a non-ergodic polar phase to an ergodic weakly polar after the applying of an electric field of 60 kV/cm⁻¹.