Structure and Oxidation Behavior of a Plasma Sprayed Yttrium Silicates Coated SiC-C/C with a Glass Outer Sealant from 1 573K to 1 873K

Different compositions of yttrium silicates coatings were deposited on SiC-C/C by plasma spraying and an outer borosilicate glass was applied on the yttrium silicates coatings surfaces.The structure of the multi-layer coatings was characterized by XRD and SEM analyses.High temperature oxidation behavior of the multi-layer coatings coated C/C composites was investigated.Results show that SiC/2SiO_2Y_2O_3/I.5SiO_2 Y_2O_3/SiO_2 Y_2O_3/glass multi-layer coating has better high temperature oxidation resistance,protecting carbon/ carbon composites from oxidation at 1 773 K in air for 164 h with the weight loss of 1.65%.The oxidation weight loss of the coated C/C with time accorded with parabolic rule in the temperature range 1 573 K-1 873 K; and the corresponding oxidation activation energy of the coated carbon/carbon composites is 132.2 kJ/mol.     

碳/碳复合材料防氧化涂层研究新进展

介绍了最近几年我们制备的几种高性能的碳／碳复合材料的氧化保护涂层的结构和高温氧化行为，表明采用包埋和渗透法制备的Si—MoSi2、SiC—MoSi2、Al2O3-莫来石-SiC—Al4SiC4以及Al2O3-莫来石-SiC涂层不仅具有很好的抗热震性能，而且能够将碳／碳复合材料的高温氧化保护温度提高到1973K;此外还介绍了一些涂层的失效机理。     

SiC/Si-W-Mo coating for protection of C/C composites at 1873 K

In order to prevent carbon/carbon composites from oxidation at 1873 K, an efficient oxidation protective SiC/Si-W-Mo coating was prepared by a two-step pack cementation technique. The microstructures and the phase composition of the as-received multi-coating were examined by scanning electron microscopy （SEM） and X-ray diffraction （XRD）. It is seen that the compact multi-coating is composed of α-SiC, Si, and （WxMO1-x）Si2. Oxidation test shows that, after oxidation at 1873 K in air for 102 h and thermal cycling between 1873 K and room temperature for 10 times, the weight loss of the SiC/Si-W-Mo coated C/C composites is only 0.26%. The invalidation of the multi-coating is attributed to the formation of penetrable cracks in the coating. 2008 University of Science and Technology Beijing. All rights reserved.     

Improved oxidation resistance of chemical vapor reaction SiC coating modified with silica for carbon/carbon composites

To protect carbon/carbon (C/C) composites from oxidation, a SiC coating modified with SiO2 was prepared by a complex technology. The inner SiC coating with thickness varying from 150 to 300 μm was initially coated by chemical vapor reaction (CVR): a simple and cheap technique to prepare the SiC coating via siliconizing the substrate that was exposed to the mixed vapor (Si and SiO2) at high temperatures (1 923?2 273 K). Then the as-prepared coating was processed by a dipping and drying procedure with tetraet...     

Preparation and anti-oxidation mechanism of mullite/yttrium silicate coatings on C/SiC composites

In order to enhance the oxidation resistance of C/Si C composites, mullite/yttrium silicate coatings were fabricated on C/Si C composites through dip-coating route. Al_2O_3-SiO_2 sol with high solid content was selected as the raw material for mullite and "silicone resin + Y_2O_3 powder" slurry was used to synthesize yttrium silicate. The microstructure and phase composition of coatings were characterized, and the investigation on oxidation resistance and anti-oxidation mechanism was emphasized. The as-fabricated coatings consisting of SiO_2-rich mullite phase and Y_2Si_2O_7 phase show high density and favorable bonding to C/Si C composites. After oxidized at 1 400 ℃ and 1 500 ℃ for 30 min in static air, the coating-containing C/Si C composites possess 91.9% and 102.4% of the original flexural strength, respectively. The desirable thermal stability of coatings and the further densification of coatings due to viscous flow of rich SiO_2 and Y-Si-Al-O glass are responsible for the excellent oxidation resistance. In addition, the coating-containing composites retain 99.0% of the original flexural strength and the coatings exhibit no cracking and desquamation after 12 times of thermal shock from 1 400 ℃ to room temperature, which are ascribed to the combination of anti-oxidation mechanism and preferable physical and chemical compatibility among C/Si C composites, mullite and Y_2Si_2O_7. The carbothermal reaction at 1 600 ℃ between free carbon in C/Si C substrate and rich SiO_2 in mullite results in severe frothing and desquamation of coatings and obvious degradation in oxidation resistance.     

Influence of deposition voltage on phase, microstructure and antioxidation property of cristobalite aluminum phosphate coatings

Cristobalite aluminum phosphate (C-AlPO₄) coatings were prepared by a hydrothermal electrophoretic deposition process on SiC-coated C/C composites. Phase compositions and microstructures of the as-prepared coatings were characterized by XRD and SEM analyses. The influence of deposition voltage on the phase, microstructure and antioxidation property of the cristobalite aluminum phosphate coatings was investigated. Results show that the as-prepared coatings are composed of cristobalite aluminum phosphate crystallites. The thickness and density of cristobalite aluminum phosphate coatings are improved with the increase of deposition voltage. The deposition amount and bonding strength of the cristobalite aluminum phosphate coatings also increase with the increase of deposition voltage. The deposition mass per unit area of the coatings and the square root of the deposition time at different hydrothermal voltages satisfy linear relationship. The antioxidation property of the coated C/C composites is improved with the increase of deposition voltage. Compared with SiC coatings prepared by pack cementation, the multilayer coatings prepared by pack cementation with a later hydrothermal electrophoretic deposition process exhibit better antioxidation property. The as-prepared multi-coatings can effectively protect C/C composites from oxidation in air at 1 773 K for 37 h with a mass loss rate of 0.53%.     

Influence of deposition voltage on phase, microstructure and antioxidation property of cristobalite aluminum phosphate coatings

Cristobalite aluminum phosphate (C-AlPO4) coatings were prepared by a hydrothermal electrophoretic deposition process on SiC-coated C/C composites. Phase compositions and microstructures of the as-prepared coatings were characterized by XRD and SEM analyses. The influence of deposition voltage on the phase, microstructure and antioxidation property of the cristobalite aluminum phosphate coatings was investigated. Results show that the as-prepared coatings are composed of cristobalite aluminum phosphate crystallites. The thickness and density of cristobalite aluminum phosphate coatings are improved with the increase of deposition voltage. The deposition amount and bonding strength of the cristobalite aluminum phosphate coatings also increase with the increase of deposition voltage. The deposition mass per unit area of the coatings and the square root of the deposition time at different hydrothermal voltages satisfy linear relationship. The antioxidation property of the coated C/C composites is improved with the increase of deposition voltage. Compared with SiC coatings prepared by pack cementation, the multilayer coatings prepared by pack cementation with a later hydrothermal electrophoretic deposition process exhibit better antioxidation property. The as-prepared multi-coatings can effectively protect C/C composites from oxidation in air at 1 773 K for 37 h with a mass loss rate of 0.53%.     

Microstructure and properties of SiC gradiently coated Cf/C composites prepared by a RCLD method

The SiC gradiently coated carbon fiber/carbon (Cf/C) composites were prepared by a two-step rapid chemical liquid depo-sition (RCLD) method. The microstructure and properties of the composites were investigated using X-ray diffraction, scanning elec-tron microscopy together with energy dispersive X-ray analysis, bending tests, and oxidation tests. The experimental results show that the surface layer of the composites is composed of SiC, pyrocarbon, and carbon fibers. Their inner area consists of pyrocarbon and carbon fibers. The SiC content gradiently decreases with increasing distance from the outer surface to the center of the compos-ites. Furthermore, the thickness of the SiC layer increases with increasing tetraethylorthosilicate content and deposition time. SiC coatings have no significant influence on the bending strength of the composites. However, the oxidation resistance of the compos-ites increases with increasing thickness of the SiC layer.     

Investigation on plasma-sprayed ZrO_2 thermal barrier coating on nickel alloy substrate

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Effect of oxidation on fracture toughness of a carbon/carbon composite

The fracture toughness of a carbon/carbon composites oxidized at different temperature for 1 h was measured. The fracture surfaces were examined by scanning electron microscopy (SEM). The results indicate that oxidation temperature has significant effects on the fracture toughness. Fracture toughness decreases with the increase of the weight loss. The SEM images reveal that the decrease of fracture toughness was mainly attributed to the oxidation of the interface in the composite.     

Mechanical properties with high temperature and the microstructure of carbon/phenolic ablative composites

Carbon fiber reinforced phenolic based composites were prepared by laminating molding. The variation in mechanical characteristics of composites was evaluated with heating temperature and procedure. The microstructures of composites at different temperatures were observed by optical microscope and scanning electron microscope, respectively. The results showed that the main weight loss range of carbon/phenolic is from 300 to 800 ℃, before 700 ℃ the weight loss was resulted from pyrolysis and after that the weight loss was mainly by oxidation in the fiber phase; with the heat treatment temperature rising, the bonding at the interface of carbon fibers and resin matrix weakened; in the pyrolysis temperature range, the interlaminar shear strength(ILSS) of carbon/phenolic showed a rapid drop with temperature rising, and then decrease in the rate of ILSS became relatively slower; the fiber oxidation had little influence on the ILSS.     

Synthesis of Li2Fe0.9Mn0.1SiO4/C composites using glucose as carbon source

Li2Fe0.9Mn0.1SiO4/C composites were synthesized by using glucose as carbon source. The samples were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and electrochemical measurements. All Li2Fe0.9Mn0.1SiO4/C composites are of the similar crystal structure. With increasing the carbon content in the range of 5%-20% (mass fraction), the diffraction peaks in XRD patterns broaden and the particle sizes and the tap density of samples decrease. The Li2Fe0.9Mn0.1SiO4/C composites with carbon content of 14.12% show excellent the capacity retention remains 92.2% after 30 cycles.     

不同含量的活性元素钇对K38高温合金1000℃氧化行为的影响

研究添加不同含量活性元素钇（Y）的K38铸造高温合金在1 000℃的氧化行为.结果表明：不添加活性元素Y合金的氧化质量增加明显高于含Y合金.不添加Y的合金和添加0.05%（质量分数,以下同）Y的合金发生了内氧化,内氧化物为Al2O3和TiN.而含0.1%和0.5%Y的合金没有内氧化发生,Y促进了Al的选择性氧化.当Y含量达0.5%时,合金中析出富Y相,降低了合金的氧化抗力.     

碳/碳生物活性玻璃涂层复合材料的组织结构研究

通过包埋－粉末涂刷高温烧结工艺，以碳化硅作为过渡层制备出C／C生物活性玻璃涂层复合材料。采用SEM、EDS、XRD考察了涂层的组织结构，结果表明所制涂层具有多孔结构，从基体到生物活性玻璃涂层，成分和结构呈连续变化，消除了生物玻璃与基体的性质差异，实现了在C／C复合材料表面进行生物活性改性。     

不同前驱体制备的Al/K碳烟燃烧催化剂的催化性能

以Al(NO3)3(或Al2O3)和KNO3(或KOH)为原料,采用直接涂抹法,制取不同比例的Al/K碳烟催化剂。通过程序升温氧化(TPO)研究了焙烧温度、老化时间对催化剂催化活性的影响,同时用XRD对催化剂的成分进行分析。结果表明,Al/K摩尔比为3∶1、1∶1和3∶1的Al2O3/KNO3,Al(NO3)3/KNO3和Al2O3/KOH催化活性都较高。但是,高温焙烧或老化时,由于降低催化剂的比表面积导致催化剂催化活性明显降低;Al2O3/KOH经过焙烧形成K2Al2O4,故表现出较好的催化活性,但是吸水能力较强。     

水热温度对碳/碳复合材料表面HAp/壳聚糖生物复合涂层的影响

以声化学法合成的纳米羟基磷灰石(HAp)为起始原料,以异丙醇作为分散介质,采用水热电泳沉积法在经壳聚糖(CS)溶液改性后的碳/碳复合材料(C/C)表面沉积HAp/CS生物复合涂层.重点研究水热温度对复合涂层晶相、形貌的影响及涂层的沉积动力学机理.采用X射线衍射仪(XRD)、透射电子显微镜(TEM)、傅立叶变换红外光谱分析仪(FTIR)和扫描电子显微镜(SEM)对所制备的涂层进行表征.结果表明:随着水热温度的升高,涂层表面由微晶疏松结合的多孔结构向紧密结合的多孔结构转变,涂层的内聚力增强;涂层的沉积速率随水热温度的升高而增加,涂层的沉积活化能为43.58 kJ/mol.     

TiO2/碳纳米管复合材料的氧化热失重特性及动力学

对采用水热合成法制备的TiO2/碳纳米管复合材料,进行了氧化热失重和动力学分析。考察了升温速率和TiO2负载量对于热失重(TG)和差示扫描(DSC)曲线的影响。结果表明,升温速率的增加会使TG和DSC曲线向高温区稍有偏移,而TiO2负载量的增加会使TG和DSC曲线向低温区明显偏移,但两者对TiO2/碳纳米管复合材料的最终转化率并无影响。采用Kissinger和Ozawa非等温法进行了氧化热失重反应的拟合,得到了十分相近的表观活化能和频率因子,线性回归系数R2均在0.99以上,拟合效果较为理想。     

The Mixed-Alkali Effect on The Resistance of Glass to Water

Based on the composition of float glass, the resistance of glass to water, in which a small amount of K2O (0-1.0 wt% ) was substituted for equivalent amount of Na2O, was investigated by means of glass grains testing. The components extracted from the glass and total alkalinities in extraction solution were determined by atomic absorption spectroscopy and neutralizing method, respectively. The composition of the glass was 14.4 K2O Na2O, 4.0MgO, 8.2CaO, 1.4Al2 O3, 72.0 SiO2, and the minimum extraction ratio of oxides (maximum durability) occurred at a K2 O/Na2O ratio of 0.051( by weight) due to the presence of the mixed-alkali effect. The relative extraction ratio of alkali oxides (R2O) was greater than that of alkaline earth oxides (RO) . By means of mixed-alkali effect and lowing relative contents of R2O in the glass, the resistance of float glass to water was improved and its mildew-proof ability was therefore increased.     

Electrical resistance behavior of vinylester composites filled with glass-carbon hybrid fibers

Vinylester (bismethacryloxy derivative of a bisphenol-A type EP resin, VE) composites with glass-carbon hybrid fibers (CF-GF) weight fraction of 50%, were prepared by the compress molding method. The distribution of carbon fiber in the hybrids was observed by stereomicroscope. The electrical resistance behavior of the composites filled with different carbon fiber (CF) weight contents (0.5% to 20%) was studied. The experimental results show that the electrical resistance behaviors of CF-GF/VE composites are different with those of CF/VE composites because carbon fibers’ conducting networks are broken by the glass fibers in the CF-GF/VE composites. The carbon fibers distribute uniformly in the networks of glass fibers (GF) like single silk and form the semi-continuous conducting networks. Composite filled with GF-CF hybrid has a higher percolation threshold than that filled with pure CF. At that time, the resistivity of CF-GF/VE composites varies little with the temperature increasing. The temperature coefficient of resistivity in GF-CF/VE composite is less than 317 ppm and the variation of the resistivity after ten thermal cycles from 20 °C to 240 °C is less than 1.96%. Funded by the Natural Science Foundation of Hubei Province (No. 2007ABA028)     

Magneli phase titanium sub-oxide conductive ceramic Ti_nO_(2n-1) as support for electrocatalyst toward oxygen reduction reaction with high activity and stability

Magneli phase titanium sub-oxide conductive ceramic Tin O2n-1 was used as the support for Pt due to its excellent resistance to electrochemical oxidation, and Pt/Tin O2n-1 composites were prepared by the impregnation-reduction method. The electrochemical stability of Tin O2n-1 was investigated and the results show almost no change in the redox region after oxidation for 20 h at 1.2 V(vs NHE) in 0.5 mol/L H2SO4 aqueous solution. The catalytic activity and stability of the Pt/Tin O2n-1 toward the oxygen reduction reaction(ORR) in 0.5 mol/L H2SO4 solution were investigated through the accelerated aging tests(AAT), and the morphology of the catalysts before and after the AAT was observed by transmission electron microscopy. At the potential of 0.55 V(vs SCE), the specific kinetic current density of the ORR on the Pt/Tin O2n-1 is about 1.5 times that of the Pt/C. The LSV curves for the Pt/C shift negatively obviously with the half-wave potential shifting about 0.02 V after 8000 cycles AAT, while no obvious change takes place for the LSV curves for the Pt/Tin O2n-1. The Pt particles supported on the carbon aggregate obviously, while the morphology of the Pt supported on Tin O2n-1 remains almost unchanged, which contributes to the electrochemical surface area loss of Pt/C being about 2times that of the Pt/Tin O2n-1. The superior catalytic stability of Pt/Tin O2n-1 toward the ORR could be attributed to the excellent stability of the Tin O2n-1 and the electronic interaction between the metals and the support.