两步法制备具有自愈合能力的纯SiC涂层

为了提高碳/碳(C/C)复合材料的抗氧化性能,通过两步法在基体表面制备了具有自愈合能力的纯SiC涂层.首先,通过高含氢硅油(H-PSO)的高温热解在基体表面引入SiC纳米线,然后通过高温渗Si,在碳材料表面生成厚度约为100-200μm的涂层.通过X射线衍射(XRD)、扫描电子显微镜(SEM)表征了所制备的涂层形貌及相组成,并对所制备的试样进行了氧化实验.实验结果表明:涂层是由纯SiC构成的,且具有一定的自愈合能力;所制备的试样在1400℃下氧化4h,失重仅为0.71%,抗氧化性能得到提高.     

水热温度对SiC-C/C复合材料表面水热电泳沉积MoSi2抗氧化涂层的影响

采用水热电泳沉积法和固相渗透法在C/C复合材料表面制备了MoSi2/SiC复合抗氧化涂层。分别采用X射线衍射、扫描电子显微镜和等温静态氧化实验对复合涂层的晶相组成、显微结构和抗氧化性能进行了表征。主要研究了水热电泳沉积温度对MoSi2外涂层显微结构及高温抗氧化性能的影响,重点分析了涂层试样在1500℃和1630℃下的静态氧化行为及失效机理。结果表明:外涂层主要由MoSi2和少量MoO3晶相组成。外涂层的致密程度、厚度及抗氧化性能随着水热温度的升高而提高。MoSi2/SiC复合涂层具有较好的抗氧化和抗热震能力,在1 500℃下有效保护基体320 h同时经历17次1 500℃与室温之间的热循环后,氧化失重率仅为1.07%;在1630℃下氧化88 h后失重率为2.17%。复合涂层在1 630℃下的氧化失效主要是由于经过长时间氧化后SiO2玻璃膜层不能及时有效填补涂层中的缺陷,涂层试样在热循环过程中产生了贯穿性的孔洞导致的。     

莫来石抗氧化外涂层的制备及抗氧化性能

以莫来石粉体(3Al2O3·2SiO2)为原料,采用水热电泳沉积法在C/C-SiC复合材料表面制备了莫来石外涂层。借助XRD和SEM等对涂层的晶相组成和显微结构进行了表征。研究了水热沉积电压对莫来石外涂层相组成、形貌及高温抗氧化性能的影响。结果表明:外涂层主要由莫来石晶相组成。当沉积电压控制在120~180 V范围内时,莫来石外涂层的致密程度、厚度及抗氧化性能随着沉积电压的升高而提高。当沉积电压达到210 V时,制备的外涂层出现疏松、裂纹等缺陷,抗氧化性能减弱。抗氧化测试表明与包埋法制备的SiC-C/C涂层试样相比,莫来石-SiC-C/C涂层试样的抗氧化性能明显提高。当沉积电压为180 V时,制备的复合涂层试样可在1500℃的空气气氛下有效保护C/C复合材料164 h,其失重仅为1.75%。     

微波水热时间对C/C复合材料结构和抗氧化性能的影响

以磷酸、B4C和Al2O3为原料,采用一种新的微波水热法对C/C复合材料基体进行了抗氧化改性,重点研究了微波水热时间对改性试样物相组成、微观结构和抗氧化性能的影响。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能量色散谱仪(EDS)及X射线光电子能谱(XPS)对改性后试样进行了表征。结果表明:改性后复合材料表面覆盖了一层由熔融态的HPO3、B2O3和结晶的Al(PO3)3、微量B4C粒子组成的涂层。经60~120 min的微波水热改性,复合材料的抗氧化性能随着微波水热处理时间的延长而改善,达到一定程度后,其变化不再明显。微波水热处理100 min后的试样抗氧化性能最佳,在600℃静态空气气氛下氧化16 h后,氧化失重仅为9.5×10-4 g.cm-2,氧化失重速率维持在4.46×10-5 g.cm-2.h-1的极低水平。     

水热沉积电压对ZrSiO4抗氧化涂层显微结构及抗氧化性能的影响

以硅酸锆粉体为原料,异丙醇为溶剂,碘为荷电介质,采用水热电泳沉积法在C/C-SiC复合材料基体表面制备了硅酸锆外涂层。通过X射线衍射(XRD)、扫描电子显微镜(SEM)对涂层的晶相结构和微观形貌进行表征。研究了水热电泳沉积电压对涂层的显微结构及高温抗氧化性能的影响,并分析了涂层试样在1 773 K下静态空气中的氧化行为。结果表明：电泳沉积电压在160~200 V范围内,复合涂层的致密程度、厚度及抗氧化性能随着沉积电压的升高而提高。但沉积电压过高(220 V),复合涂层中出现微裂纹等缺陷,此时涂层的抗氧化性能下降。沉积电压控制在200 V时所制备的复合涂层可在1 773 K静态空气中有效保护C/C复合材料332 h,氧化失重率仅为0.2%,相应的氧化失重速率稳定在48.3 μg·cm^-2·h^-1的极低水平。     

C/C,C/C-SiC梯度基、纳米基、双元基复合材料微观结构特征

采用C和SiC共沉积的CVI技术制备了C/C ,C/C SiC梯度基、纳米基和双元基复合材料 .用光学显微镜、电子探针微观分析、透射电子显微镜和扫描电子显微镜观察了各种材料微观结构 .结果表明 ,SiC加入到碳基体里改变了热解碳的微观结构并导致了C/C复合材料性能的改善 .每种材料都各具特点 .由于它们密度低、良好的力学性能和抗氧化性能使得这些材料成为很有希望的热结构复合材料     

铜粒子负载泡沫基相变复合材料的制备与性能

以三聚氰胺泡沫(MF)经高温碳化后制得的碳泡沫(CF)为基体, 以氯化铜(CuCl₂)和水合肼(N₂H₄·H₂O)溶液为前驱体, 利用氧化还原反应在泡沫骨架上生成铜粒子, 然后通过真空浸渍法将聚乙二醇(PEG)封装在基体中制得相变复合材料. 利用扫描电子显微镜(SEM)、 X射线衍射仪(XRD)、 差示扫描量热仪(DSC)和红外热成像仪等研究了相变复合材料的形貌、 结构和热性能. 结果表明, 当CuCl₂浓度为1.0 mol/L时, Cu粒子均匀致密地沉积在CF骨架表面, 制得的相变复合材料在具备良好密封性能的前提下, 相变潜热可高达145.2 J/g, 热效率超过80%, 光热转换效率达到83.8%, 且呈现出优异的储热能力和调温性能. 本文为制备综合性能优异的相变复合材料提供了一种策略, 有利于拓宽相变复合材料的应用领域.     

新型ACNT/C纳米复合材料氧化性能的初步研究

以定向碳纳米管阵列为骨架, 利用化学气相渗(CVI)工艺制备了新型的定向碳纳米管/炭(ACNT/C)纳米复合材料, 并对其氧化性能进行了初步的研究. SEM形貌观察表明, 氧化后的ACNT/C纳米复合材料仍然保持着其基本的管状结构特点, 氧化由外层热解炭向内逐渐进行. 热失重分析 (TGA)检测结果表明, 密度为0.80 g•cm-3的ACNT/C纳米复合材料在空气中的热失重转变温度约为720 ℃, 比相同工艺条件下制备的密度为1.5 g•cm-3的C/C复合材料提高了50 ℃左右. 静态空气等温氧化实验表明, ACNT/C纳米复合材料在550 ℃氧化过程中的化学反应速率明显低于C/C复合材料. 这主要是由于ACNT/C纳米复合材料具有稳定的界面和较高的晶化程度.     

钙熔盐电解石墨阳极破损机理及防护研究

通过扫描电镜和电子探针分析钙熔盐电解中破损石墨阳极的结构和杂质,探索了其破损机理,认为主要是由于孔隙存在导致氧化和孔隙吸附电解质,电解质因水解、脱水等过程使其周围的石墨阳极颗粒受应力不平衡而发生破损.通过实验研制出适合于钙熔盐电解过程用的石墨阳极具有抗氧化性能的涂层,并对涂层进行了XRD,SEM分析和氧化失重实验.实验表明该涂层在680～750℃下成硼玻璃态,能渗透到石墨阳极孔隙中,涂层表面致密无裂纹且附着力强,因而具有较好的抗氧化能力.该涂层是一种适合钙熔盐电解的、性能优良的石墨阳极涂层.     

金属载体表面氧化及预载处理对氧化铝涂层结合性能的影响

对FeCrAl基体进行高温氧化后,再浸渍MgAl2O4/Al2O3过渡涂层,利用XRD、 SEM和超声波振动等方法研究了样品的表观性质和涂层的结合性能.结果表明,一定时间的氧化处理可以在金属基体上形成粗糙的表层,增加涂层粘结的表面积.共沉淀法制备的尖晶石前驱体凝胶反应活性大,可作为粘结剂掺入浆料中,制备均匀的MgAl2O4/Al2O3过渡涂层.在金属载体表面氧化及预载处理后,可采用传统浸渍工艺负载γ-Al2O3分散涂层,并保证涂层的结合力.     

Surface characteristic and cell response of CVD SiC coating for carbon/carbon composites used for hip arthroplasty

SiC coatings were applied on carbon/carbon composites by chemical vapor deposition for potential application in hip arthroplasty. The surface morphology, roughness, and wettability of the coatings were evaluated by scanning electron microscopy, laser confocal scanning microscope, and video‐based contact angle measuring device, respectively. The bonding strength between the coatings and carbon/carbon composites was analyzed by scratch testing. The cell responses to coatings were studied by analyzing the cell morphology and cell proliferation. The results showed that SiC coatings showed spherical morphology with a roughness of R_a = 1.0 ± 0.2 µm and a contact angle of 64.7 ± 4.0°. The coatings had lower surface roughness and better surface hydrophilicity compared with those of the uncoated carbon/carbon composites. A strong shear strength averaging 120.0 MPa between the coating and carbon/carbon composites was achieved. The cell culture experiments showed that cell spreading was improved, and cell proliferation was increased with the SiC coatings. It was demonstrated that CVD‐SiC‐coated carbon/carbon composites were good candidates as artificial hip joint materials. Copyright © 2012 John Wiley & Sons, Ltd.     

Influence of MoSi2 content in suspension on the phase, microstructure and properties of hydrothermal electrophoretic deposited SiC n �CMoSi2 coating for SiC pre-coated C/C composites

To protect carbon/carbon (C/C) composites from oxidation at high temperature, a nano SiC?CMoSi₂ (SiC _n ?CMoSi₂) coating on SiC pre-coated C/C composites was prepared by hydrothermal electrophoretic deposition. The phase composition, surface and cross-section microstructures of the prepared SiC _n ?CMoSi₂ coating deposited with different MoSi₂/SiC _n mass ratio were characterized by X-ray diffraction (XRD), energy-dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). The influence of MoSi₂ content in the hydrothermal electrophoretic deposition suspension on the phase composition, microstructure and high-temperature oxidation resistance of the multi-layer coatings were investigated. Results showed that the content of MoSi₂ phase in the prepared coating increases with the increase of MoSi₂ content in the suspension. The density and oxidation resistance of the SiC_n-MoSi₂ coating improve with the increase of MoSi₂ mass content from 20 to 60 wt% in the deposition suspension. However, micro-cracks and micro-holes in the coating are found when deposited with 80 wt% MoSi₂, and a decrease in oxidation resistance was also detected. The multi-layer coatings deposited with suspension of 60 wt% MoSi₂ exhibited the best anti-oxidation ability, which can effectively protect C/C composites from oxidation in air at 1,873 K for 90 h with weight loss of 2.08%.     

用Raman光谱研究碳纤维/聚醚醚酮复合材料的界面结构

用Ｒａｍａｎ光谱研究碳纤维／聚醚醚酮复合材料的界面结构李铁骑章明秋曾汉民（中山大学材料科学研究所聚合物复合材料及功能材料国家教委开放研究实验室广州５１０２７５）关键词界面结构，Ｒａｍａｎ光谱，碳纤维／聚醚醚酮复合材料随着近年来热塑性聚合物的加工...     

Design of oxidation-resistant coatings for high-temperature composites

Fabrication of oxidation-resistant carbon fiber reinforced carbon composites requires use of high-temperature CVD deposition of coatings such as SiC. In this paper the use of low-temperature chemical approaches for depositing oxidation-resistant coatings was explored. Coatings of SiO₂, B₂O₃, and SiC were examined, with the intent of distinguishing possible failure mechanisms. Factors contributing to poor oxidation resistance of these coatings include presence of microcracks in the original preparation of the coating and diffusion of oxygen through the coating at high temperatures.     

Ablation properties of C/C–SiC composites tested on an arc heater

Carbon fiber-reinforced carbon and silicon carbide (C/C–SiC) composites were fabricated by a combination of chemical vapor infiltration and liquid silicon infiltration. Ablation properties of C/C–SiC composites and C/C composites with similar technique were tested on a high-pressure arc heater. The results show that ablation properties of C/C–SiC composites are more severe than those of C/C composites. Ablation of C/C–SiC composites includes oxidation, sublimation of SiC (Si), and mechanical denudation. Oxidation and sublimation of SiC (Si) lead to the enlarged ablation rates between carbon fibers and matrices, which finally cause serious ablation of C/C–SiC composites.     

Electrophoretic deposition of nickel, iron and aluminum nanoparticles on carbon fibers

The electrophoretic deposition (EPD) of nickel (Ni), iron (Fe) and aluminum (Al) nanoparticles fabricated by an active hydrogen plasma evaporation method on the surface of carbon fibers was investigated, which will allow the obtained composites to be applied as practical catalysts or electrodes. SEM observations show that the Ni nanoparticles can build up a thick EPD coating with some cracks on the surface of carbon fibers, and the analyses of X-ray diffraction (XRD) and BET specific surface area indicate that fine particles from the as-received Ni powders were finally deposited after the EPD process without crystal growth. The surface oxidation of Fe and Al nanoparticles takes serious effect on the EPD process and the morphology of the as-prepared coatings.     

Applying diamond like carbon layer on carbon/carbon composites and its effect on the deposition of hydroxyapatite coating

The biomedical application of carbon/carbon (C/C) composites is limited by lacking bioactivity and releasing carbon debris. Hydroxyapatite (HA) coating has been used to improve the bioactivity of C/C composites, but it cannot reduce the release of carbon debris effectively because of poor wear resistance property. In this work, a wear‐resistant layer of diamond like carbon (DLC) is applied on C/C composites, followed by an ultrasound‐assisted electrochemical deposition to prepare HA coatings. The microstructure, morphology and chemical composition of the DLC layer and the HA coating are characterised by scanning electron microscopy, X‐ray diffraction, energy dispersive spectroscopy (EDS), X‐ray photoelectron spectroscopy, Fourier transformed infrared spectroscopy and Raman spectrum. The bonding strength between the HA coating and the DLC layer modified C/C composites is examined by a tensile test. The results show that the DLC layer has a spherical morphology and provides a uniform surface for the deposition of the HA coating. The HA coating shows flaky morphology with a compact structure. The tensile strength of the HA coating on the DLC layer modified C/C composites is 6.24 ± 0.40 MPa, which is significantly higher than that of HA coating on unmodified C/C composites(3.04 ± 0.20 MPa). Copyright © 2013 John Wiley & Sons, Ltd.     

Nano/micro‐sized calcium phosphate coating on carbon/carbon composites by ultrasonic assisted electrochemical deposition

Nano/micro‐sized calcium phosphate (CaP) coating was prepared on carbon/carbon (C/C) composites by ultrasonic assisted electrochemical deposition. The coating obtained at different deposition voltages contained a mixture of hydroxyapatite (HA) and brushite (DCPD). The homogenous coating prepared at 2.4 V consisted of nano‐sized and needle‐like HA embedded in micro‐sized and plate‐like DCPD. An interlocking structure was formed along the depth direction of the coating. The internal stress may be released effectively through the interlocking structure of the coating. And the plate‐like crystals of the coating were inset in the grooves on the surface of C/C composites. This led to a better adhesive strength of the coating. Meanwhile, the formed interlocking structure could help enhance cohesive strength of the coating. It was found that the growth of CaP crystals in the coating under the voltage of 2.4 V consisted of the plate‐like crystals deposited initially. Then the plate‐needle‐like crystals of submicron size formed among the plate‐like crystals and developed needle‐like ones. The CaP‐coated C/C composites might improve the biological properties of coating for its unique morphology, structures and strong adhesion to the C/C substrate. Copyright © 2011 John Wiley & Sons, Ltd.