XPS,AFM研究沥青基碳纤维电化学表面处理过程的机制

对各向同性沥青基碳纤维进行电化学氧化表面处理,用XPS,AFM分析了碳纤维表面含氧官能团和表面微观形貌的变化过程。实验结果表明:电化学氧化处理是表面碳及其含氧官能团逐步被氧化成羧基和CO₂的过程。氧化处理首先是使碳纤维表面变得更光滑,持续氧化后才会出现沟槽,SEM的分辨率不足以表征碳纤维电化学氧化前后的表面形貌变化,而采用AFM可在纳米尺度上表征碳纤维在电化学氧化过程中的表面形貌变化。AFM和XPS的结合可表征碳纤维电化学氧化表面处理的进程。     

低温等离子体碳纤维表面处理技术研究

采用低温等离子体法对碳纤维表面进行处理,并通过滴水试验、SEM、XPS测试处理效果。与阳极氧化法相比,低温等离子体法能更有效地改变碳纤维的表面性质。滴水试验表明经等离子体处理的碳纤维表面呈极性,与水的润湿性好;SEM测试结果表明,低温等离子体法处理的碳纤维表面沟槽比阳极氧化法的更多,前者表现出更强的表面修饰性;XPS测试结果表明,经等离子体和阳极氧化法处理后的碳纤维表面均含有羧基、羟基、羰基,低温等离子体处理后的碳纤维表面的极性官能团总含量为17%。     

AZ-1改性炭纤维/聚三唑复合材料界面研究

研究了一种用氮丙啶处理炭纤维的方法在新型聚三唑树脂复合材料中的界面作用效果和作用机理.用硝酸氧化处理炭纤维,再引入分子结构中含氮丙啶环的化合物AZ-1,通过化学手段对炭纤维进行改性.结果表明,经改性后炭纤维增强聚三唑树脂复合材料比未处理复合材料的层间剪切强度提高86%.AFM,SEM和接触角测试表明化学改性增加了炭纤维...     

碳纤维改性对不饱和聚酯自修复复合材料性能的影响

采用H_2O_2和浓HNO_3对碳纤维(CF)表面分别进行氧化处理,得到氧化碳纤维(OCF1和OCF2),采用硅烷偶联剂γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)对OCF1进行接枝处理,得到接枝改性碳纤维(KCF),将改性前后CF应用于不饱和聚酯(UP)自修复复合材料中,分析比较了不同改性剂及改性方法对碳纤维/不饱和聚酯(CF/UP)自修复复合材料性能的影响。利用FTIR、XPS、SEM表征CF与CF/UP自修复复合材料的化学结构与形貌,通过TGA、万能拉力试验机、悬臂梁冲击仪、邵氏硬度计等对复合材料的热稳定性、力学性能及自修复效率进行测试。结果表明:氧化、接枝反应均可增加CF表面的粗糙度和活性官能团含量,从而改善CF与UP基体的界面相容性。其中OCF1/UP自修复复合材料的综合力学性能比OCF2/UP自修复复合材料好,KCF/UP自修复复合材料的力学性能在三者之中最佳,其自修复效率最高,可达67.03%。     

氧化法提高碳纤维增强复合材料强度的研究

采用扫描电子显微镜和Ｘ射线光电子能谱仪对经高温氧化处理的碳纤维表面的形貌和活性基团进行研究,并用处理过的纤维制成纤维增强复合材料试样,进行了强度试验及断口分析,同时讨论了氧化法提高纤维和树脂间界面结合强度的机制。     

KH-570接枝改性碳纤维/乙烯-醋酸乙烯共聚物复合泡沫材料的制备及表征

采用浓H₂SO₄/浓HNO₃混合酸对碳纤维(CF)进行表面氧化处理得到氧化碳纤维(OCF),再利用γ-甲基丙烯酰氧丙基三甲氧基硅烷(KH-570)与OCF进一步反应得到KH-570接枝改性碳纤维(KCF),随后将其应用于乙烯-醋酸乙烯共聚物(EVA)复合泡沫材料中。利用FTIR、XPS、Raman、FESEM和电子万能试验机等考察了碳纤维的表面改性效果以及碳纤维/EVA复合材料的结构与性能。结果表明:氧化和接枝反应均可以增加碳纤维表面的活性官能团含量和粗糙度,从而改善碳纤维与EVA基体之间的相容性,使碳纤维/EVA复合泡沫材料的物理性能得到改善。相同条件下,KH-570接枝改性碳纤维/EVA复合泡沫材料的物理性能更优异。      

电化学氧化处理对PAN基炭纤维表面浸润性的影响

以硫酸铵为电解质,对炭纤维进行连续电化学氧化处理,利用反气相色谱(IGC)研究电化学氧化处理前后的表面能变化,并联系SEM、AFM、XRD、Raman、XPS等测试结果综合分析电化学氧化处理对炭纤维表面性能的影响。研究表明,经电化学氧化处理后,纤维沿轴方向表面沟槽加深加宽,薄弱层被剥除,晶格择优取向遭到破坏;纤维表面活性官能团增多,氧和氮含量分别增加了180%和65%,提高了纤维与树脂的粘结性;纤维表面能提高了3.1倍,与树脂的浸润性得到改善;电化学氧化处理后其复合材料的ILSS达109MPa,已可充分满足实际应用需求。     

阳极氧化对炭纤维电镀镍的影响

采用阳极氧化法对炭纤维进行连续表面改性,并在其表面进行电镀镍处理,利用扫描电子显微镜(SEM)、X射线衍射(XRD)、热重分析和酸碱滴定等方法研究了炭纤维阳极氧化前后的物理化学结构及对炭纤维电镀镍镀层的影响。结果表明:经过阳极氧化处理后,炭纤维表面的总酸性官能团提高约10倍;炭纤维拉伸强度降低先慢后快;阳极氧化可以改善镀层的生长过程,使镍镀层的生长由(V-W)模式转变为(F-M)模式,并且促使镀层晶粒细晶化,N i晶粒尺寸由14.5nm降为11.2nm,提高了镀镍炭纤维的抗氧化性以及镀层与炭纤维的结合力,阳极氧化后镀镍的炭纤维初始氧化温度较镀镍炭纤维提高了50℃。     

Influence of fibre surface oxidation–reduction followed by silsesquioxane coating treatment on interfacial mechanical properties of carbon fibre/polyarylacetylene composites

Carbon fibre was treated with oxidation–reduction followed by silsesquioxane coating method to improve the interfacial properties of carbon fibre/polyarylacetylene (CF/PAA) composites. The treatment method was divided into three phases, i.e., oxidation with oxygen plasma, reduction with LiAlH₄, and coating treatment with vinyl silsesquioxane (VMS–SSO). The fibre surface composition and functional group were analyzed using X-ray photoelectron spectroscopy (XPS). The polar functional groups, especially C–OH which could react with Si–OH on silsesquioxanes, were increased after redox reaction. VMS–SSO coating treatment imported vinyl groups which could react with PAA resin during PAA cure process. The surface morphology of carbon fibre was observed by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The mechanical interfacial properties of the CF/PAA composites were characterized by short-beam bending testing method. Interlaminar shear strength (ILSS) of the CF/PAA composites in different treatment phases were increased by 31.7%, 28.8%, and 59.3%, respectively. The conclusion that oxidation–reduction followed by silsesquioxane coating treatment is an effective method to improve the interfacial properties of the CF/PAA composites can be drawn. This method can be used in other resin systems if the functional groups on silsesquioxane are changed according to those in resins.     

低密度碳粘接碳纤维复合材料(CBCF)抗氧化改性研究

以全氢聚硅氮烷(PHPS)为原料, 采用浸渍-热转化方法, 在低密度碳粘接碳纤维复合材料(CBCF)中短切碳纤维表面成功包覆硅氧氮(SiON)涂层。采用扫描电子显微镜(SEM)、能量色散X射线光谱(EDS)等分析测试手段对碳纤维表面的SiON涂层进行了形貌和物相分析, 结果表明: 涂层主要由Si、O、N元素组成, 在PHPS浓度为3wt%和5wt%条件下制备的涂层均匀、致密, 随着PHPS浓度的提高, 涂层厚度增加, 但易发生结块。当PHPS浓度为10wt%和20wt%时, 制备的SiON涂层出现结块并且存在裂纹。采用热重分析和等温氧化实验对纯CBCF和SiON涂层改性的CBCF复合材料抗氧化性能进行考核, 结果显示碳纤维表面包覆SiON涂层能够显著提高CBCF复合材料的抗氧化性, 随着PHPS浓度增大, 低密度CBCF复合材料抗氧化性能显著提高。     

Highly conductive polymer materials based multi-walled carbon nanotubes as counter electrodes for dye-sensitized solar cells

Poly(3,4-ethylenedioxxythiophene) (PEDOT), polyaniline (PANI) and polythiophene (PTh) based multi-walled carbon nanotube (MWCNT) composites were successfully prepared using RF-rotating plasma grafting method. Morphological characterizations of composites were determined using scanning electron microscopy (SEM), which showed that conducting polymers (CPs) of PEDOT, PANI and PTh were coated on the surface of CNTs. The surface properties of the Carbon Nanotube (CNT) composites were also determined by using Infrared Spectra (FT-IR), X-ray Photon Spectra (XPS), and Scanning Electron Microscopy-Energy Dispersive X-ray Spectra (SEM-EDX) analysis. X-ray photon spectra results confirmed the formation of the composites. Composites of MWCNT were used in dye-sensitized solar cells (DSSCs) as counter electrodes and exhibited short-circuit photocurrent densities of 11.19, 10.70 and 8.54 mA/cm² for PANI/MWCNT, PTh/MWCNT and PEDOT/CNT, respectively.     

聚合物涂层对高模量碳纤维表面性能的影响

为改善碳纤维表面性能以及碳纤维/树脂复合材料的界面性能,对PAN基高模量碳纤维（HMCF）表面进行聚合物涂层处理。研究了不同潜伏性固化剂含量的聚合物涂层对HMCF表面以及碳纤维/树脂复合材料的界面性能的影响。IR分析表明,聚合物涂层与纤维或树脂基体发生了化学反应。扫描电镜和动态机械热分析的结果也说明,聚合物涂层能够提高...     

国产聚丙烯腈基高强高模碳纤维电化学氧化表面处理工艺

以国产聚丙烯腈（PAN）基M55J级碳纤维（CF）为研究对象,首先在不同电解液体系中进行循环伏安多重扫描,比较其氧化能力的差异,进行电解液的筛选。然后用最佳电解液对CF进行恒流连续氧化处理,通过Raman光谱、XPS和SEM的表征,研究了电化学氧化对高强高模CF表面结构及化学组成的影响,并通过测试CF束丝拉伸性能及其与树脂结合后的层间剪切强度对CF的力学性能进行了表征。研究结果表明,NH₄HSO₄电解质溶液对CF进行表面处理时,其刻蚀能力最强,可以有效改善其表面活性,增大其表面粗糙度和含氧官能团数量。采用0.6 mol/L的NH₄HSO₄电解液体系,在1 mAcm^-2电流密度下对CF进行阳极氧化,CF与树脂间的层间剪切强度比未处理提高了164%,同时CF的拉伸强度略有提高,模量无明显变化。     

MoSi2-SiC 抗氧化涂层对碳/碳复合材料弯曲性能的影响

在C/C 复合材料表面制备了MoSi₂-SiC 抗氧化涂层, 分析了涂层工艺对C/C 复合材料组织的影响, 测试了材料的室温弯曲力学性能。结果表明, 该工艺在C/C 复合材料表面生成抗氧化涂层的同时, 基材内部的层间和纤维束界面, 以及孔隙周围也被硅化。C/C 复合材料经涂层工艺处理后, 弯曲断裂行为发生改变, 弯曲强度明显升高,塑性有一定程度的降低。      

电子束固化树脂基复合材料中碳纤维表面改性研究

利用阳极氧化方法和偶联剂对碳纤维表面的物理和化学性质进行改性，采用原子力显微镜（AFM）和X射线光电子能谱（XPS）分析了碳纤维表面改性前后的形貌和化学成分的变化，利用Keaelble法计算了碳纤维的表面能。研究结果表明，阳极氧化改性的碳纤维表面粗糙度增加，表面活性；表面活性官能闭增多，表面能中极性成分增加明显，碳纤维表面引入的活性氮和化学吸附的碱性物质使电子束固化复合材料界面处的引发剂中毒，复合材料界面性能减弱，与电子束固化工艺相匹配的偶联剂在碳纤维与树脂基体之间形成化学桥，使电子束固化复合材料界面性能得到明显提高。     

Study on surface and mechanical fiber characteristics and their effect on the adhesion properties to a polycarbonate matrix tuned by anodic carbon fiber oxidation

Polyacrylonitrile (PAN) based high strength carbon fibers were anodically oxidized using the galvanostatic mode in alkaline electrolyte solutions to influence the chemical surface composition. The change of chemical and physical properties was investigated using scanning electron microscopy (SEM), photoelectron spectroscopy (XPS), energy dispersive X-ray analysis (EDX) and contact angle as well as zeta (ζ)-potential measurements.

An initially improved wettability for polar liquids, particularly water, was observed for oxidized carbon fibers. This result was confirmed by ζ-potential measurements. The chemical state of the oxygen containing surface groups changes during anodic oxidation in K₂CO₃/KOH due to further oxidation of C–OH and C=O groups to COOH groups. Therefore the surface acidity increases, which leads to a shift of the isoelectric point to lower pH values and increases the negative ζ_plateau value. The ζ–pH as well as the ζ–concentration dependence show the same tendency. During anodic oxidation of carbon fibers in KNO₃/KOH electrolyte solution beside ‘normal’ (like C–OH, C=O and COOH) surface oxides also carboxylate groups (COO⁻K⁺) were formed at the fiber surface in contrast to an oxidation in K₂CO₃/KOH which introduces ‘normal' surface oxides. No influence could be observed of such an anodic oxidation on the single fiber tensile strength. Contact angle measurements of polycarbonate melt droplets onto single carbon fibers show no dependence of the surface composition. The interfacial shear strength, measured using the microdroplet pull-off test were compared with the thermodynamic work of adhesion. The calculated as well as the measured adhesion show the same absence of any influence of fiber treatment.     

SiC涂层/三维碳纤维编织体的氧化动力学和机理研究

采用原位反应法在三维碳纤维编织体(简称:RB)的纤维表面制得SiC涂层,通过 XRD、SEM、等温氧化失重和非等温热重分析等测试手段研究了制备方法对SiC涂层均匀性 的影响,并对SiC涂层／碳纤维编织体(简称:CB)材料在等温和非等温条件下,氧化反应的 动力学和反应机理进行了研究.结果表明:SiC涂层均匀、完整地涂覆于编织体内外各纤维表 面;材料等温氧化反应的机理为第一阶段反应控制,第二阶段扩散和反应共同控制;材料的非 等温氧化过程呈现自催化特征,氧化机理为随机成核,氧化动力学参数为:lgA=9.615min^-1; E_a=201.73kJ·mol^-1.     

炭纤维表面官能团异氰酸酯化及阴离子接枝尼龙6研究--(Ⅰ)接枝方法与表征

提出了炭纤维(CF)表面接枝的一种新方法。通过CF表面官能团的异氰酸酯化,利用异氰酸酯作为MC尼龙6聚合的活化剂,成功地通过阴离子接枝聚合方法制备了表面接枝尼龙6(PA6)的CF。扫描电子显微镜(SEM)结果表明．接枝了PA6的CF表面呈粗颗粒状形态与织构。X光光电子能谱(XPS)结果表明阴离子接枝PA6的CF表面N／C比例由0．0295提高到0．0573。称量法表明接枝率可达1．8％以上。     

Microarc oxidation coating formed on SiCw/AZ91 magnesium matrix composite and its corrosion resistance

A ceramic coating was synthesized on the surface of SiCw/AZ91 magnesium matrix composite by means of microarc oxidation (MAO) technique. Scanning electron microscope (SEM) was employed to characterize the surface morphology and cross-section microstructure of the coating. The phase structure and the chemical composition of the ceramic coating were analyzed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The corrosion resistance of the coating was evaluated by immersion test and electrochemical method. The results showed that the corrosion rate of the coated SiCw/AZ91 composite was decreased greatly compared with that of the bare composite because of the protective microarc oxidation coating.     

复合处理碳纤维增强聚酰亚胺复合材料力学性能

采用浓硝酸氧化和聚酰亚胺(PI)包覆复合方法对短切碳纤维(CF)进行表面改性,提高CF增强热塑性聚酰亚胺复合材料(CF/TPI)力学性能。采用比表面积及孔容分析、原子力显微镜、扫描电子显微镜、热重分析仪研究了CF表面处理前后结构和形貌的变化。结果表明：CF经浓HNO₃处理后比表面积增加144.2%,CF表面沟壑加深;复合处理后有PI层包覆在 CF表面;包覆处理后CF耐热性能提高。力学性能测试表明,经过包覆处理后CF/TPI复合材料的拉伸强度比未处理的提高11.34%,弹性模量提高109.2%,弯曲强度提高18.78%,冲击强度提高74.15%。