Synthesis and characterization of Yb and Er based monosilicate powders and durability of plasma sprayed Yb2SiO5 coatings on C/C-SiC composites

Rare-earth silicates such as Yb₂SiO₅ and Er₂SiO₅ are promising environmental barrier coating materials for ceramic matrix composites. In this work, Yb₂SiO₅ and Er₂SiO₅ ceramic powders have been synthesized by solid-state reaction using Yb₂O₃, Er₂O₃ and SiO₂ as starting materials. The fabricated powders were subjected to spray drying treatment for subsequent synthesis of coatings by plasma spraying. The spray drying resulted in well-dispersed and spherical powder particles with good flowability. Analytical techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetry and differential scanning calorimetry (TGA/DSC) and dilatometry were applied to study the microstructural and thermal characteristics of the powders. Ultra-high purity monosilicate powders formed as a result of heating treatments at 1400 °C in a box furnace for 20 h. TG/DSC revealed the genesis temperatures of the silicate formation (low temperature polymorphs) and also showed that the solid-state reactions to form Yb and Er based monosilicates proceeded without any weight-loss in the tested temperature range. The values of coefficients of thermal expansion (CTE) of the fabricated compounds are found to be 7.1 ppm/°C for Yb₂SiO₅ and 7.5 ppm/°C for Er₂SiO₅ by dilatometric measurements. Besides these studies, coating formation by plasma spraying of spray-dried Yb₂SiO₅ powders on the ceramic matrix composite specimen such as C/C-SiC has also been evaluated. Well-adhered and uniformed coatings result on composite specimens whose durability is tested by thermal cycling from ∼400 °C to 1500 °C in a gas burner rig.     

Synthesis of Fe/SiO2 composite particles and their superior electromagnetic properties in microwave band

Fe/SiO₂ composite particles were synthesized by hydrogen reduction of Fe₂O₃/SiO₂ precursor, which was prepared by sol-gel method. A reduction temperature higher than 600 °C is required for the complete conversion of Fe₂O₃ to Fe. Fe/SiO₂ composite particles exhibit superior complex permittivity and permeability in the microwave band. A reflection loss higher than − 70 dB as well as a broad absorption band can be simultaneously obtained for Fe/SiO₂-based coatings about 2 mm in thickness, suggesting that the Fe/SiO₂ composite particles are a promising candidate for high performance electromagnetic absorption materials.     

外贴Fe3O4/CNTs杂化碳纳米纸的碳纳米管复合材料吸波性能

通过对Fe₃O₄纳米粒子接枝碳纳米管的单分散水溶液真空吸滤制备出一种新型的杂化碳纳米纸, 它与树脂浸润良好, 可以与复合材料一体成型。分别借助FE-SEM、EDS、BJH法和振动样品磁强计表征杂化碳纳米纸及其复合材料的微观形貌、元素组成、平均孔径分布和磁性能。在8.2~18 GHz频段内利用波导法测量碳纳米管共混复合材料和外贴杂化碳纳米纸/碳纳米管共混复合材料的电磁参数和吸波反射率。研究结果表明: 外贴一层杂化碳纳米纸(厚0.1 mm)后, 碳纳米管共混复合材料的磁损耗明显增加, 在8.2~18 GHz微波频段内吸波反射率基本上全部小于-10 dB(频宽大于9.7 GHz), 在15.42 GHz位置, 反射损耗峰达-43.18 dB, 远优于碳纳米管共混复合材料。     

Influence of SiO2 fillers on microwave absorption properties of carbonyl iron/carbon black double-layer coatings

Epoxy resin (ER) based double-layer composite coatings were prepared with the thickness of 1.2 mm, employing carbonyl iron (CI) and carbon black (CB) as absorbents in the matching layer and absorption layer respectively. Especially, SiO₂ was introduced into the matching layer as wave-transmission material to improve the matching impendence. The complex permittivity, complex permeability and absorption properties were investigated in 2–18 GHz. With increasing SiO₂ content in the matching layer, the reflection loss (RL) was enhanced in the range 2–18 GHz. When the coating with the optimized SiO₂ and CI weight concentration (SiO₂:CI:ER) of 2:5:1, the optimal RL got to −17.3 dB and the effective absorption band (RL better than −4 dB) reached 5.7 GHz. In comparison, the minimum RL value was only −5.9 dB and the bandwidth (RL better than −4 dB) was just 4.1 GHz for the SiO₂-free composite coating.     

Electromagnetic interference shielding behavior of poly(trimethylene terephthalate)/multi-walled carbon nanotube composites

Poly(trimethylene terephthalate) [PTT]/multiwalled carbon nanotube [MWCNT] composites having varying amounts of MWCNTs were fabricated with an aim to investigate the potential of such composites as an effective light weight electromagnetic interference (EMI) shielding material in the frequency range of 12.4-18 GHz (Ku-band). PTT/MWCNT composite with shielding effectiveness (SE) of 36-42 dB was obtained at 10% (w/w) MWCNT loading. Shielding mechanism was studied by resolving the total SE into absorption (SE_A) and reflection loss (SE_R). PTT/MWCNT composite showed absorption dominated shielding; thus it can be used as microwave, radar absorbing and stealth material. The effect of MWCNT loadings on electrical conductivity (σ) and dielectric properties of PTT and the correlation among conductivity, tan δ, absorption loss and reflection loss were also studied.     

Oriented growth of magnetite along the carbon nanotubes via covalently bonded method in a simple solvothermal system

A new type of CNTs/magnetite hybrid material was prepared via covalently bonded method in a simple solvothermal system using FeCl₃ as iron source, ethylene glycol as the reducing agent, and 4-aminophenoxyphthalonitrile-grafted CNTs as templates. The magnetite nanoparticles, with the diameters of 70-80 nm, were self-assembled along the CNTs. The FTIR, UV-vis and DSC revealed that a stable covalent bond between nitriles group and iron ion promoted the oriented growth of magnetite nanoparticles along the CNTs, resulting in good dispersibility and solution storage stability. The magnetic properties measurements indicated that a higher saturated magnetization (70.7 emu g⁻¹) existed in the CNTs/magnetite hybrid material, which further enhanced the electromagnetic properties. The magnetic loss was caused mainly by natural resonance, which is in good agreement with the Kittel equation results. The novel electromagnetic hybrid material is believed to have potential applications in the microwave absorbing performances.     

Highly strong and conductive carbon nanotube/cellulose composite paper

Carbon nanotube (CNT)/cellulose composite materials were fabricated in a paper making process optimized for a CNT network to form on the cellulose fibers. The measured electric conductivity was from 0.05 to 671 S/m for 0.5–16.7 wt.% CNT content, higher than that for other polymer composites. The real permittivities were the highest in the microwave region. The unique CNT network structure is thought to be the reason for these high conductivity and permittivity values. Compared to other carbon materials, our carbon CNT/cellulose composite material had improved parameters without decreased mechanical strength. The near-field electromagnetic shielding effectiveness (EMI SE) measured by a microstrip line method depended on the sheet conductivity and qualitatively matched the results of electromagnetic field simulations using a finite-difference time-domain simulator. A high near-field EMI SE of 50-dB was achieved in the 5–10 GHz frequency region with 4.8 wt.% composite paper. The far-field EMI SE was measured by a free space method. Fairly good agreement was obtained between the measured and calculated results. Approximately 10 wt.% CNT is required to achieve composite paper with 20-dB far-field EMI SE.     

Improvement of magnetic characteristics and electrical properties of FeCoHfO/AlOx multilayered films

High permeability magnetic films can enhance the inductance of thin-film inductors in DC-DC converters. In order to obtain high permeability, effective uniaxial anisotropic field should be as low as possible. A multilayered technique (laminating the magnetic layers with oxide spacers) was exploited to improve the magnetic properties of thick films. The FeCoHfO/AlO_x multilayered films were fabricated by dc reactive magnetron sputtering. Inserting an insulator (AlO_x) layer can decrease the magneto-elastic anisotropy by reducing the residual stress of the FeCoHfO magnetic films. The anisotropic field and resistivity of the FeCoHfO/AlO_x multilayered films were evidently improved by multilayered coating. With this optimum configuration of 9 layers structure [FeCoHfO (133 nm)/AlO_x (10 nm)]₉, low anisotropic field (H_K = 65 Oe) and high resistivity (ρ ∼ 1350) μΩ cm were achieved.     

Effect of MgWO4 content on properties of Ba0.5Sr0.5TiO3 composite ceramics for tunable microwave applications

xMgWO₄-(1 − x) Ba_0.5Sr_0.5TiO₃ (x = 0.0, 5.0, 15.0, 25.0 and 35.0 wt%) composite ceramics were prepared via solid state reaction processing. Their structural and dielectric properties were systematically characterized. A significant increase in grain size was observed with increasing MgWO₄ content, which was accompanied by obvious variations in dielectric properties of the composite ceramics. It is found that the permittivity peaks of the samples gradually shifted to low temperatures with increasing MgWO₄ content. At the same time, tunabilities of the composite ceramics decreased, but their Q values increased. The sample with 35 wt% MgWO₄ possesses a high tunability of 16.8% (∼10 kHz), a low permittivity of 65 and an appropriate Q value of 309 (∼4.303 GHz), which meet the requirements of high power and impedance matching, thus making it a promising candidate for applications as electrically tunable microwave devices.     

A study of the electromagnetic properties of Cobalt-multiwalled carbon nanotubes (Co-MWCNTs) composites

Electroless plating was utilized to deposit Cobalt (Co) on the surface of multi-walled carbon nanotubes (MWCNTs), and the technological parameters of electroless plating were optimized. To obtain optimized processing parameters, field-emission scanning electron microscope (FESEM) as well as energy dispersive spectroscopy (EDS) results were presented to show the morphology, components of as-prepared Co-MWCNTs. Based on the optimized processing parameters, Co-MWCNTs were prepared and filled into the epoxy resin to fabricate Co-MWCNTs composites. The electromagnetic properties of pure MWCNTs composites and Co-MWCNTs composites were studied. To sum up, the pure MWCNTs composites with a filler concentration of 2 wt% had an intense absorbing peak at 15.20 GHz, where the highest reflection loss (R) reached −21.41 dB. Compared to the pure MWCNTs composite at the same concentration, the Co-MWCNTs composites showed a higher impedance which implies a better potential absorbing property and makes Co-MWCNTs probable to be utilized in electromagnetic absorbing field.     

High-performance ZnO thin film transistors with sputtering SiO2/Ta2O5/SiO2 multilayer gate dielectric

A high-performance ZnO thin film transistor （ZnO-TFT） with SiO₂/Ta₂O₅/SiO₂ (STS) multilayer gate insulator is fabricated by sputtering at room temperature. Compared to ZnO-TFTs with sputtering SiO₂ gate insulator, its electrical characteristics are significantly improved, such as the field effect mobility enhanced from 11.2 to 52.4 cm²/V s, threshold voltage decreased from 4.2 to 2 V, and sub-threshold swing improved from 0.61 to 0.28 V/dec. The improvements are attributed to the high gate capacitance (from 50 to 150 nF/cm²) as well as nice surface morphology by using dielectric with high～k Ta₂O₅ sandwiched by SiO₂ layers. The capacitance-voltage characteristic of a metal-insulator-semiconductor capacitor with the structure of Indium Tin Oxide/STS/ZnO/Al was investigated and the trap charges at the interface or bulk is evaluated to be 2.24 × 10¹² cm⁻². From the slope of C⁻² versus gate voltage, the doping density N_D of ZnO is estimated to be 1.49 × 10¹⁶ cm⁻³.     

Percolative property and microwave dielectric characterization of Ba0.4Sr0.6TiO3-Mg2TiO4 diphasic ceramics

Ba_0.4Sr_0.6TiO₃-Mg₂TiO₄ composite ceramics were fabricated via conventional solid state reaction process. Dielectric properties of the composites were investigated systematically. It was shown that their dielectric constants decreased monotonously from 1197 to 60 with the contents of increasing Mg₂TiO₄ from 0 to 70 wt%. Tunability had a slight change from 24.0% to 20.5% as the volume fraction of Mg₂TiO₄ was increased from 0 to 62 vol%. However, it decreased substantially from 20.5% to 13.4% above the threshold from 62 vol% to 71 vol%. Such an obvious change in tunability was well explained by connectivity levels of the binary composites. Q values of the composite ceramics were more than 200 (tg δ < 0.005) at microwave frequencies of less than 10 GHz. Dielectric dispersion was observed at about 22 GHz using interdigital capacitor (IDC) stucture.     

碳纳米管/ABS树脂基复合材料的力学性能和雷达波吸收性能的研究

采用竖式炉流动法制备的碳纳米管经液相阳极氧化表面处理后增强ABS热塑性工程塑料。复合材料的力学性能研究显示:碳纳米管的加入有效提高了复合材料的拉伸性能,但材料的耐冲击性能下降。当碳纳米管含量为12 wt%时,复合材料的拉伸强度由45.00 MPa提高到69.96 MPa,杨氏模量由0.75 GPa提高到1.93 GPa。对碳纳米管/ABS复合材料的反射系数测定表明:复合材料在一定频率范围内有雷达波吸收性能。     

Fabrication of transparent conductive carbon nanotubes/polyurethane-urea composite films by solvent evaporation-induced self-assembly (EISA)

Transparent and conductive carbon nanotubes (CNTs)/polyurethane-urea (PUU) composite films were prepared by solvent evaporation-induced self-assembly (EISA). Pristine CNTs were treated with acids (H₂SO₄/HNO₃ = 3:1, v:v), acylated with thionyl chloride, and purified after filtration. These acylated CNTs (0.05 wt.% in dimethylformamide, DMF) were deposited onto the 3-aminopropyl triethoxysilane (APTES)-modified glass substrate by DMF EISA at 100 °C with the withdrawal rate of 3 cm/h. The CNT layers of 200–400 nm thicknesses were transferred to the PUU films by solution casting or resin transfer molding (RTM) at ambient temperature. Optical transmittances of the composite films were 60–75% at 550 nm wavelength and their sheet resistances were 5.2 × 10⁰–2.4 × 10³ kΩ/square, and which varied significantly with type of CNTs and the transferring methods of CNT layers.     

The effect of carbon nanotubes microstructures on reinforcing properties of SWNTs/alumina composite

Alumina reinforced with 1 wt% single-wall carbon nanotubes (SWNTs) was fabricated by hot-pressing. The fracture toughness of SWNTs/Al₂O₃ composite reaches 6.40 ± 0.3 MPa m^1/2, which is twice as high as that of unreinforced alumina. Nanoindentation introduced controlled cracks and the damage were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SWNTs reinforcing mechanisms including CNT pullout, CNT fracture, CNT bridging and crack deflection were directly observed, and the relationship between carbon nanotubes microstructures in the matrix and mechanical properties was also discussed in detailed.     

Multi-barrier layer-mediated growth of carbon nanotubes

Variation in the height of carbon nanotubes (CNTs) grown has been co-related to the type of multi-barrier-layer used. Initially, various types of barrier-layers such as Al, Al₂O₃, Al/SiO₂, Al₂O₃/SiO₂ were prepared onto a n-type Si (100) substrate. The thickness of SiO₂ was ∼ 550 nm, where as, Al₂O₃ and Al were ∼ 15 nm thick. These samples were covered with ∼ 1 nm thick Fe catalyst layer. The coated samples were subjected to the thermal chemical vapor deposition (T-CVD) process. SEM analysis showed that, for Al₂O₃/SiO₂ barrier layers, the average height of the CNTs was ∼ 10 μm, where as, for other types of samples it was less than ∼ 1 μm. To investigate this, multi-barrier layers were characterized by dynamic secondary ion mass spectrometry (D-SIMS). The observed variation in height of CNTs is attributed to the variation in diffusivity of Fe atoms into multi-barriers-layers. The results showed that, diffusion of Fe catalyst atoms could severally affect height of CNTs.     

Preparation, dielectric and ferroelectric properties of Pb5Ge3O11 and Pb5Ge2.85Si0.15O11 thin films fabricated by sol-gel process

Lead germanate-silicate (Pb₅Ge_2.85Si_0.15O₁₁) ferroelectric thin films were successfully fabricated on Pt/Ti/SiO₂/(100)Si substrates by the sol-gel process. The thin films were fabricated by multi-coating at preheating temperatures of 350 and 450 °C. After annealing the thin films at 600 °C, the films exhibited c-axis preferred orientation. The degree of c-axis preferred orientation of the thin films preheated at 350 °C was higher than that of films preheated at 450 °C. Grain growth was influenced by the annealing time. The thin films exhibited a well-saturated ferroelectric P-E hysteresis loop when preheated at 350 °C and annealed at 600 °C for 1.5 h. The values of the remanent polarization (Pr) and the coercive field (Ec) were approximately 2.1 μC/cm² and 100 kV/cm, respectively.     

Preparation and thermoelectric properties of nc-Si:(Al2O3 + SiO2) composite film

A composite film of nanocrystalline Si (nc-Si) embedded in (Al₂O₃ + SiO₂) has been prepared on a quartz substrate by thermally evaporating a 400 nm thick Al film on a quartz substrate and annealing in air at 580 °C for 1 h. During annealing, the Al reacts with the SiO₂ of the quartz substrate and produces nc-Si, which is embedded in the (Al₂O₃ + SiO₂) film. The average size of nc-Si is ~ 22 nm and the thickness of the nc-Si:(Al₂O₃ + SiO₂) composite film is ~ 810 nm. It is found that the prepared film is thermoelectric with a Seebeck coefficient of − 624 μV/K at 293 K and − 225 μV/K at 413 K.     

Influence of carbon nanotube-polymeric compatibilizer masterbatches on morphological, thermal, mechanical, and tribological properties of polyethylene

Study was made of the effect of multiwall carbon nanotubes (MWCNTs) and polymeric compatibilizer on thermal, mechanical, and tribological properties of high density polyethylene (HDPE). The composites were prepared by melt mixing in two steps. Carbon nanotubes (CNTs) were melt mixed with maleic anhydride grafted polyethylene (PEgMA) as polymeric compatibilizer to produce a PEgMA-CNT masterbatch containing 20 wt% of CNTs. The masterbatch was then added to HDPE to prepare HDPE nanocomposites with CNT content of 2 or 6 wt%. The unmodified and modified (hydroxyl or amine groups) CNTs had similar effects on the properties of HDPE-PEgMA indicating that only non-covalent interactions were achieved between CNTs and matrix. According to SEM studies, single nanotubes and CNT agglomerates (size up to 1 μm) were present in all nanocomposites regardless of content or modification of CNTs. Addition of CNTs to HDPE-PEgMA increased decomposition temperature, but only slight changes were observed in crystallization temperature, crystallinity, melting temperature, and coefficient of linear thermal expansion (CLTE). Young’s modulus and tensile strength of matrix clearly increased, while elongation at break decreased. Measured values of Young’s moduli of HDPE-PEgMA-CNT composites were between the values of Young’s moduli for longitudinal (E₁₁) and transverse (E₂₂) direction predicted by Mori-Tanaka and Halpin-Tsai composite theories. Addition of CNTs to HDPE-PEgMA did not change the tribological properties of the matrix. Because of its higher crystallinity, PEgMA possessed significantly different properties from HDPE matrix: better mechanical properties, lower friction and wear, and lower CLTE in normal direction. Interestingly, the mechanical and tribological properties and CLTEs of HDPE-PEgMA-CNT composites lie between those of PEgMA and HDPE.     

The effect of MgO and SiO2 codoping on the properties of Nd:YAG transparent ceramic

Nd:YAG transparent ceramics were fabricated by a reactive sintering method under vacuum using SiO₂, MgO and compound additives (SiO₂ and MgO) as sintering aids. The effects of SiO₂ and MgO on the microstructure and sintering process of Nd:YAG ceramics were studied. High quality Nd:YAG ceramics with compound sintering aids obtained by vacuum sintering at 1780 °C are composed of grains of the size ∼10 μm, and their transmittance is 82% at 400 nm. It was found the absorption coefficient of 1.0 mol% Nd:YAG ceramic was 8.6 cm⁻¹ at 808 nm and its absorption cross section was calculated to be 6.26 × 10⁻²⁰ cm².