Thermal conductivity and thermal cycle life of La2O3 and HfO2 doped ZrO2-Y2O3 coatings produced by EB-PVD

The effects of La₂O₃ and HfO₂ addition on thermal conductivity and thermal cycle life of EB-PVD YSZ coatings were investigated. La₂O₃ and HfO₂ were selected as additives, because they significantly suppress the sintering of YSZ. The developed coating showed low thermal conductivity as well as high resistance to sintering. Burner rig tests confirmed that the developed coating have a superior thermal insulating effect and have a longer life than that of a coating with conventional composition.     

氨基功能化CoFe2O4-SiO2 磁性复合材料的制备及其在去除水中重金属离子的吸附性能

钴-铁氧体纳米粒子(CoFe₂O₄ NPs)通过改良的共沉淀法制备,CoFe₂O₄-SiO₂磁性复合材料通过st?ber法合成,为了吸附重金属离子CoFe₂O₄-SiO₂进行了氨基功能化。这种吸附剂的晶体结构、形貌、颗粒尺寸、化学组成和分子结构采用X射线衍射图谱(XRD)、扫描电子显微镜(SEM)以及傅里叶变换红外光谱(FTIR)进行表征。此复合材料具有优良的磁性能,由于其高的饱和磁化强度,磁铁可以将其在30秒内快速分离。同时,CoFe₂O₄ NPs的磁性能可以通过烧结温度进行调节,随烧结温度提高,磁性能增强。溶液的pH及反应时间对重金属离子吸附的影响进行了研究,此外此吸附剂对Cu (II)、Cd (II)、Mn (II) 和Zn (II)具有较高的吸附容量和去除率,这一结果使此复合材料可以潜在应用于废水中重金属离子的吸附上。     

High-frequency magnetic properties of FeNi3-SiO2 nanocomposite synthesized by a facile chemical method

Monodisperse core-shell structured FeNi₃-SiO₂ composite nanoparticles (NPs) were synthesized by a facile hydrazine reduction combined modified Stöber method. SEM and TEM analysis shows that FeNi₃ cores are composed of small primary nanocrystals and are coated by amorphous SiO₂ layer. As-prepared FeNi₃-SiO₂ nanocomposites exhibit typical soft magnetic properties. The permeability spectra vary with the contents of SiO₂. When the SiO₂ content is 10 wt%, the real part μ′ of the permeability reaches about 10 and is almost independent of frequency in the frequency range up to 1 GHz. And the imaginary part μ′′ remains very low. This paper presents a facile approach to fabrication of novel soft magnetic materials for high-frequency applications.     

Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Cyclic oxidation behavior and thermal barrier effect of YSZ-(Al2O3/YAG) double-layer TBCs prepared by the composite sol-gel method

Novel YSZ (6 wt.% yttria partially stabilized zirconia)-(Al₂O₃/YAG) (alumina-yttrium aluminum garnet, Y₃Al₅O₁₂) double-layer ceramic coatings were fabricated using the composite sol-gel and pressure filtration microwave sintering (PFMS) technologies. The thin Al₂O₃/YAG layer had good adherence with substrate and thick YSZ top layer, which presented the structure of micro-sized YAG particles embedded in nano-sized α-Al₂O₃ film. Cyclic oxidation tests at 1000 °C indicated that they possessed superior properties to resist oxidation of alloy and improve the spallation resistance. The thermal insulation capability tests at 1000 °C and 1100 °C indicate that the 250 μm coating had better thermal barrier effect than that of the 150 μm coating at different cooling gas rates. These beneficial effects should be mainly attributed to that, the oxidation rate of thermal grown oxides (TGO) scale is decreased by the “sealing effect” of α-Al₂O₃, the “reactive element effect”, and the reduced thermal stresses by means of nano/micro composite structure. This double-layer coating can be considered as a promising TBC.     

SiO_2含量对激光熔覆含La_2O_3生物陶瓷涂层性能的影响

采用激光熔覆技术,利用CaHPO_4·2H_2O,CaCO_3,La_2O_3,SiO_2粉末和Ti粉在医用钛合金Ti-6Al-4V表面制备掺杂的质量分数分别为0%,5%,10%,15%SiO2的含La2O3梯度生物陶瓷涂层,并研究了SiO_2含量对涂层性能的影响。利用金相显微镜、扫描电镜、能谱仪、X射线分析仪分别对涂层进行显微结构、表面元素、物相组成分析,利用MTT细胞活性检测法对涂层上种植的小鼠破骨前体细胞(RAW264.7)进行细胞活性分析。结果显示:掺杂10%~15%的SiO_2后,涂层的裂纹明显减少,且厚度变均匀。涂层在模拟体液(SBF)中浸泡2周后,羟基磷灰石(HA)在掺杂10%SiO_2涂层表面的沉积量最多,涂层表面的金属元素含量稀少,这表明含10%SiO_2涂层在SBF中具备更加优良的沉积HA的能力,同时有效的阻碍了基体中重金属离子的析出。MTT结果表明,掺杂SiO_2的涂层对破骨前体细胞的活性有更加明显的抑制作用。     

MoS2颗粒表面包覆Al2O3及其在镀层中的应用

采用非均匀形核法将Al2O3包覆到MoS2颗粒表面,提高颗粒的亲水性能。研究了溶液pH值、Al(NO3)3的摩尔浓度和预处理工艺对包覆率的影响;采用SEM及EDS分析了包覆前后MoS2颗粒的微观形貌和表面成分;通过测量接触角研究了颗粒表面的亲水性。结果表明,颗粒表面均匀包覆了一层Al(OH)3;溶液pH值对包覆率的影响最大,Al(NO3)3的摩尔浓度次之。最佳工艺为:溶液pH值为5.5,Al(NO3)3浓度为0.15mol/L,预处理过程不添加表面活性剂。随着包覆率的提高,MoS2颗粒的亲水性提高。利用包覆Al2O3的MoS2制得了Ni-P-MoS2化学复合镀层,提高了镀层中沉积粒子的均匀致密性。     

Electrochemical performance of SiO2-coated LiFePO4 cathode materials for lithium ion battery

The surface of LiFePO₄/C particles was coated with SiO₂ via a sol-gel method, and the electrochemical performance of SiO₂-coated LiFePO₄ cathode materials at room temperature and 55 °C was investigated. Compared with pristine LiFePO₄, the structure of LiFePO₄ with SiO₂ coating had no change, the existence of SiO₂ coating effectively enhanced the cycling capacity, reduced capacity fading at high temperature and alleviated the cell impedance. The SiO₂ coating played a regulatory role for Li-ion inserting the lattice, by increasing the order of lithium ion intercalating the outer lattice of the particle. As a consequence, capacity retention improves significantly.     

Improvement in the properties of nickel by nano-Cr2O3 incorporation

Nano-ceramic composite coatings were prepared by the electrodeposition method using sulphamate electrolyte. Nickel was chosen as the metal matrix and nano-Cr₂O₃ particles were chosen as the reinforcement. The surface morphology and the particle distribution in the coating were analysed using field emission scanning electron microscope (FESEM). The particle content was obtained using energy dispersive X-ray analysis (EDAX). A change in the surface morphology of Ni was seen on the incorporation of Cr₂O₃ particles. The coatings were characterized for their structure and no change in the diffraction pattern was seen between plain Ni and Ni-Cr₂O₃ composite. The mechanical property like microhardness and tribological behaviour of the nano-composite coatings was studied and it was observed that the incorporation of Cr₂O₃ particles enhanced the mechanical properties of Ni matrix. The nano-composites were analysed for their thermal stability and corrosion resistance. An improvement in thermal stability was observed but no change in the corrosion behaviour of Ni was seen on the incorporation of nano chromium oxide particles.     

SiON/SiO2复合膜层对太阳能电池阵板间电缆的表面改性及其耐空间环境性能

在空间站工作的太阳电池阵板间电缆上下表面为聚酰亚胺薄膜,在低轨运行时会受到原子氧的强烈侵蚀,需要采取措施对其进行保护。采用射频磁控溅射法在电缆表面制备了颗粒尺寸均匀、排列致密的SiO₂膜层。通过表征空间环境试验前后样品发现由于电缆表面的凸起颗粒等缺陷无法完全被SiO₂膜层覆盖,导致原子氧会对缺陷位置产生侵蚀作用。采用全氢聚硅氮烷溶液对板间电缆基底进行表面改性处理,制备的聚硅氧氮烷涂层（SiON）可以有效地覆盖电缆基底表面的凸起颗粒等缺陷,使得其上溅射的SiO₂膜层表面光滑平整。经原子氧暴露试验,SiON/SiO₂层内部没有受到其侵蚀作用,可以防止原子氧对电缆基底的破坏。经多次冷热循环试验,SiON/SiO₂复合膜层仍然具备良好的结构特性与结合性能。     

超音速等离子喷涂工艺参数对 Cr2O3涂层硬度的影响

目的研究影响超音速等离子喷涂Cr2O3涂层硬度的主要因素,制备出高硬度涂层。方法首先采用单变量法研究超音速等离子生成气体压力(空气压力)和喷涂距离对涂层显微结构的影响,然后采用正交试验研究喷涂电流、空气压力、喷涂距离对Cr2O3涂层硬度的影响。结果工艺参数对Cr2O3涂层硬度影响的主次顺序为:空气压力>喷涂电流>喷涂距离。结论获得高硬度涂层的最佳工艺参数组合为:空气压力0.4 MPa,喷涂电流270 A,喷涂距离200 mm。在该工艺条件下获得的涂层致密、均匀,孔隙率小。     

基于磁过滤技术的热障涂层表面Al2O3 覆盖层抗CMAS腐蚀性能

为了提高热障涂层（TBC）的抗沉积物（主要成分为CaO、MgO、Al₂O₃和SiO₂,简称CMAS）腐蚀性能,采用磁过滤阴极真空电弧（FCVA）技术在TBC表面上制备了致密的Al₂O₃覆盖层,比较和分析了Al₂O₃改性TBC和沉积态TBC的润湿行为和抗CMAS腐蚀性能。结果表明：使用FCVA技术制备Al₂O₃覆盖层的过程对7%（质量分数）氧化钇稳定的氧化锆（7YSZ）相的结构无明显影响,且经Al₂O₃改性的TBC综合性能均优于沉积态TBC。在1250 ℃、CMAS腐蚀条件下,Al₂O₃覆盖层有效地限制了熔融CMAS在TBC表面上的扩散行为。同时,Al₂O₃填充了7YSZ柱状晶之间的间隔并且阻碍了熔融CMAS的渗透,证明了FCVA可作为一种制备Al₂O₃涂层的新方法以提高TBC的抗CMAS腐蚀性能,且Al₂O₃涂层及其制备过程对TBC的热震性能均无消极影响。     

Thermite reduction of Ta2O5/SiO2 powder mixtures for combustion synthesis of Ta-based silicides

Tantalum silicides (including TaSi₂, Ta₅Si₃, Ta₂Si, and Ta₃Si) were prepared by solid state combustion of the Ta-Si reaction system involving thermite reduction of Ta₂O₅ and SiO₂. The thermite-based combustion is self-sustaining and contributes to the in situ formation of tantalum silicides along with Al₂O₃. The combustion front temperature and propagation velocity increased with the extent of thermite reactions for the systems adopting the thermite mixture of Al-Ta₂O₅, while both of them decreased for those using Al, Ta₂O₅, and SiO₂ as the thermite reagents. Among four silicide compounds, a better degree of phase evolution was observed for TaSi₂ and Ta₅Si₃ when compared to that of Ta₂Si and Ta₃Si. The XRD analysis indicated the presence of a small amount of Ta₅Si₃ in the TaSi₂-Al₂O₃ composite. On the formation of Ta₅Si₃ with Al₂O₃, the minor phase was Ta₂Si for the Al-Ta₂O₅-containing system. In addition to Ta₂Si, an intermediate phase TaSi₂ was detected when the Al-Ta₂O₅-SiO₂ mixture was used. However, combustion yielded comparable amounts of Ta₂Si and Ta₅Si₃ in the synthesis of the Ta₂Si-Al₂O₃ composite. Moreover, instead of forming Ta₃Si the reaction produced Ta₂Si as the dominant phase along with unreacted Ta.     

Improvement in the corrosion resistance of TiB2/A356 composite by molten-salt electrodeposition and anodization

This study reported a novel treatment to improve the corrosion resistance of TiB₂/A356 composites. The method was employed in combination of the molten-salt electrodeposition and subsequent electrochemical anodization technique. By means of molten-salt electrodeposition, the Al coatings were deposited on the surface of TiB₂/A356 composites. It was found that the morphology of the Al coatings is closely related to the current density. Thus, under the suitable condition, a dense and uniform Al coating can be obtained, with the crystal size in the range of 0.5–2 μm and the coating thickness of ~ 9 μm. This continuous Al layer can eliminate the adverse corrosion contribution of TiB₂ particles in Al matrix. The following step of anodization was designed to convert the Al film to an anodized Al oxide film for further corrosion protection. The electrochemical corrosion behavior was evaluated by potentiodynamic polarization curves and electrochemical impedance spectroscopy. These results showed the corrosion resistance was greatly enhanced in TiB₂/A356 composites with an anodized Al-coating than that of the anodized composites. It is evident that the new treatment of metal electrodeposition in molten salts and following anodization is an effective method of anti-corrosion in composites.     

Spark plasma sintering of B4C ceramics: The effects of milling medium and TiB2 addition

Boron carbide (B₄C) ceramics, with a relative density up to 98.4% and limited grain growth, were prepared at 1600-1800 °C by spark plasma sintering (SPS) technique. The effects of powder milling medium (water and 2-propanol) on the powders' surface characteristics and TiB₂ addition on the sintering densification were investigated. The ball milling processing of B₄C powders in water can promote the sintering of B₄C ceramics. A B₂O₃ layer on B₄C particle surface is concluded to promote the densification of the B₄C ceramics at an early sintering stage. This B₂O₃ layer, which normally inhibits the densification process at the final stage of the sintering, can be reduced through reaction with TiB₂ particles, resulting in further densification of the B₄C ceramics.     

Fe3O4/SiO2/Bi2WO6磁性复合光催化剂的制备及其光催化性能

钨酸铋(Bi₂WO₆),结构最简单的Aurivillius相化合物,是近期受到研究者关注的新型光催化材料。然而,光催化剂粉末在反应介质中难被回收,工业化应用成本较高。本文用三步方法合成了可回收的Fe₃O₄/SiO₂/Bi₂WO₆磁性复合光催化剂,通过溶剂热法合成具有磁性的Fe₃O₄,用溶胶凝胶法在Fe₃O₄表面覆盖SiO₂层,后将磁性颗粒与Bi₂WO₆纳米片相结合。光催化剂的形貌结构及性能通过XRD、SEM、PL、UV-vis进行表征测试。结果表明,直径约500 nm的Fe₃O₄微球附着在边长约500 nm的Bi₂WO₆纳米片的表面,SiO₂在两者之间起到了粘连作用。光催化剂Fe₃O₄/SiO₂/Bi₂WO₆对于罗丹明B的光降解活性较好,且有一定磁性,可以通过外加磁场将其从溶液中分离,有较大的应用潜力。     

玻璃Cr2O3陶瓷涂层表面液态重金属润湿角的测量与表征

金属材料的腐蚀性能与其表面润湿特性有着密切的关系。采用亚音速火焰喷涂技术制备了玻璃-Cr2O3陶瓷涂层,设计了一套运行在高温环境中且密封的专用试验平台,研究经过不同保温时间后,重金属在45钢与喷有玻璃-Cr2O3陶瓷涂层的45钢表面的润湿角及相关现象的变化。结果表明:相同质量的重金属液滴在45钢表面的润湿角为18°,在玻璃-Cr2O3陶瓷涂层表面的润湿角为114°,玻璃-Cr2O3陶瓷涂层抗液态重金属润湿性能较好。固化后重金属颗粒与试样之间的接触面积及剪切强度均有所不同,304不锈钢与颗粒剪切强度为1.42MPa,而涂层与颗粒剪切强度为0.21MPa。     

Electroless ternary Ni-W-P alloys containing micron size Al2O3 particles

In the present investigation electroless ternary NiWP-Al₂O₃ composite coatings were prepared using an electroless nickel bath. Second phase alumina particles (1 µm) were used to codeposit in the NiWP matrix. Nanocrystalline ternary NiWP alloys and composite coatings were obtained using an alkaline citrate based bath which was operated at pH 9 and temperature at 88 ± 2 °C. Mild steel was used as a substrate material and deposition was carried out for about 4 h to get a coating thickness of 25 ± 3 µm. Metallographic cross-sections were prepared to find out the coating thickness and also the uniform distribution of the aluminum oxide particles in NiWP matrix. Surface analysis carried out on both the coatings using scanning electron microscope (SEM) showed that particle incorporation in ternary NiWP matrix has increased the nodularity of composite coatings compared to fine nodular NiWP deposits. Elemental analysis of energy dispersive X-ray (EDX) results showed that codeposited P and W elements in plain NiWP deposit were 13 and 1.2 wt.%, respectively. There was a decrease in P content from 13 to 10 wt.% with a marginal variation in the incorporated W (1.01 wt.%) due to the codeposition of aluminum oxide particles in NiWP matrix. X-ray diffraction (XRD) studies carried out on as-plated deposits showed that both the deposits are X-ray amorphous with a grain size of around 3 nm. Phase transformation studies carried out on both the coatings showed that composite coatings exhibited better thermal stability compared to plain NiWP deposits. From the XRD studies it was found that metastable phases such as NiP and Ni₅P₂ present in the composite coatings heat treated at major exothermic peak temperature. Annealed composite coatings at various temperatures revealed higher microhardness values compared to plain NiWP deposits.     

Novel thermal barrier coatings based on La2Ce2O7/8YSZ double-ceramic-layer systems deposited by electron beam physical vapor deposition

Novel thermal barrier coatings based on La₂Ce₂O₇/8YSZ double-ceramic-layer (DCL) systems, which were deposited by electron beam physical vapor deposition (EB-PVD), were found to have a longer lifetime compared to the single layer La₂Ce₂O₇ (LC) system, and even much longer than that of the single layer 8YSZ system under burner rig test. The DCL coating structure design can effectively alleviate the thermal expansion mismatch between LC coating and bond coat, as well as avoid the chemical reaction between LC and Al₂O₃ in thermally grown oxide (TGO), which occurs above 1000 °C as determined by differential scanning calorimetry (DSC) analysis. The failure mechanism of LC/8YSZ DCL coating is mainly due to the sintering of LC coating surface after long-term thermal cycling.     

Photocatalytic performance of nano-photocatalyst from TiO2 and Fe2O3 by mechanochemical synthesis

Nano-particles of homogeneous solid solution between TiO₂ and Fe₂O₃ (up to 10 mol%) have been prepared by mechanochemical milling of TiO₂ and yellow Fe₂O₃/red Fe₂O₃/precipitated Fe (OH)₃ using a planetary ball mill. Such novel solid solution cannot be prepared by conventional co-precipitation technique. A preliminary investigation of photocatalytic activity of mixed oxide (TiO₂/Fe₂O₃) on photo-oxidation of different organic dyes like Rhodamine B (RB), Methyl orange (MO), Thymol blue (TB) and Bromocresol green (BG) under visible light (300-W Xe lamp; λ > 420 nm) showed that TiO₂ having 5 mol% of Fe₂O₃ (YFT1) is 3-5 times higher photoactive than that of P25 TiO₂. The XRD result did not show the peaks assigned to the Fe components (for example Fe₂O₃, Fe₃O₄, FeO₃, and Fe metal) on the external surface of the anatase structure in the Fe₂O₃/TiO₂ attained through mechanochemical treatment. This meant that Fe components were well incorporated into the TiO₂ anatase structure. The average crystallite size and particle size of YFT1 were found to be 12 nm and 30 ± 5 nm respectively measured from XRD and TEM conforming to nanodimensions. Together with the Fe component, they absorbed wavelength of above 387 nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe₂O₃/TiO₂ particle attained through mechanochemical method. This meant that Fe components were well inserted into the framework of the TiO₂ anatase structure. EPR and magnetic susceptibility show that Fe³⁺ is in low spin state corresponding to μ_B = 1.8 BM. The temperature variation of μ_B shows that Fe³⁺ is well separated from each other and does not have any antiferromagnetic or ferromagnetic interaction. The evidence of Fe³⁺ in TiO₂/Fe₂O₃ alloy is also proved by a new method that is redox titration which is again support by the XPS spectrum.