Current status of interface modification of carbon fiber cement-based composite materials
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摘要: 碳纤维增强水泥基复合材料(Carbon fiber reinforced cement composite，CFRCC)以其高强度质量比、耐腐蚀性和耐久性而通常用于建筑、基础设施和土木工程等领域。对CFRCC而言，界面是联系基体与增强相的桥梁，界面性能、结构直接关系到复合材料粘结强度，从而直接影响到复合材料的各项宏观性能。然而，碳纤维的疏水性及其与水性悬浮液之间不充分的结合行为，限制了碳纤维在水泥和其他矿物建筑材料中的应用。为了解决这一问题，学者们研究了物理和化学改性方法，以加强从矿物基质到碳纤维的负载转移。本文介绍了碳纤维、CFRCC及CFRCC界面的性能及存在的问题。总结了近些年国内外学者对CFRCC及其界面改性方法，例如氧化、电泳沉积、等离子体和接枝处理等表面改性方法，并讨论了相关机制分析。还介绍了碳纤维本身的特性及其与水泥基质的结合行为的表征方法。Abstract: Carbon fiber reinforced cement composite (CFRCC) is widely used in the fields of construction, infrastructure, and civil engineering due to its high strength-to-weight ratio, corrosion resistance, and durability. In the context of CFRCC, the interface plays a crucial role as it acts as a bridge connecting the matrix and the reinforcing phase. The performance and structure of the interface directly impact the bond strength of the composite material, thereby influencing its overall macroscopic properties. However, the inherent hydrophobic nature of carbon fibers and their inadequate bonding with aqueous suspensions limit their application in cement and other mineral building materials. To address this issue, researchers have explored physical and chemical modification methods to enhance the transfer of load from the mineral matrix to the carbon fibers. This paper provides an overview of the properties of carbon fibers, CFRCC, and CFRCC interfaces, while also summarizing recent studies by domestic and foreign scholars on CFRCC and its interface modification methods, such as oxidation, electrophoretic deposition, plasma, and grafting treatments, along with discussions on relevant mechanistic analyses. Additionally, it presents characterization methods for studying the properties of carbon fibers themselves and their bonding behavior with cementitious matrices.
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图 1 拉伸破坏机制：(a) 连接平行于纤维轴的两个晶粒的取向错误的晶粒；(b) 平行于纤维轴施加的拉伸应力导致基面在La方向上断裂，裂纹沿着La和Lc发展；(c) 应力的进一步施加导致取向不良的微晶完全失效[58]
Figure 1. Mechanism of tensile failure: (a) Misoriented crystallite linking two crystallites parallel to fibre axis; (b) Tensile stress exerted parallel to fibre axis causes basal plane rupture in direction La, crack develops along La and Lc; (c) Further exertion of stress causes complete failure of misoriented crytallite[58]
图 2 碳纤维增强水泥基复合材料(CFRCC)的力学性能：(a) CFRCC弯曲强度与碳纤维质量分数之间的关系[65]；(b) CFRCC抗压强度与碳纤维质量分数之间的关系[65]；(c) 碳纤维对大理石灰和底灰混合料固化28天和56天抗硫酸盐性能的影响[66]
Figure 2. Mechanical properties of carbon fiber reinforced cement composite (CFRCC): (a) Relationship between CFRCC flexural strength and carbon fiber mass fraction[65]; (b) Relationship between CFRCC compressive strength and carbon fiber mass fraction[65]; (c) Effect of carbon fiber on sulfate resistance for marble dust and bottom ash mixture groups at 28 days and 56 days of curing[66]
MD—Marble dust; BA—Bottom ash; F—Carbon fibers
图 3 CFRCC的功能性：(a) 碳纤维混凝土的电阻率随碳纤维长度和含量的变化[65]；(b) 水泥基传感器中理论传导路径的示意图[3]
Figure 3. Functionality of CFRCC: (a) Electrical resistivity of CFRCC varies with carbon fiber length and content[65]; (b) Schematic presentation of theoretical conduction pathways in a cement-based sensor[3]
EDLs—Electrical double layers; Schematic presentation of theoretical conduction pathways in a cement-based sensor. The insulative cement matrix and aggregates are represented by grey and orange areas, respectively: ${\overrightarrow J _1} $—Current density in the EDLs of cement-electrolyte interface; ${\overrightarrow J _2} $ and ${\overrightarrow J _3} $—Current densities in the EDLs of fibre-electrolyte interface; ${\overrightarrow J _4} $—Current density in bulk electrolyte; ${\overrightarrow J _5} $—Current density in or between fibre bodies. For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.
图 5 (a) 臭氧改性聚乙烯(PE)纤维示意图[86]；(b) 等离子体氧化碳纤维的成键原理[87]；(c) 涂层法改性碳纤维原理示意图[91]；(d) 电化学沉积法改性碳纤维装置示意图[33]；(e) 接枝法改性碳纤维原理示意图[81]；(f) 浸渍碳纤维装置图[103]
Figure 5. (a) Ozone modified polyethylene (PE) fiber[86]; (b) Bonding principle of plasma oxidation of CF[87]; (c) Schematic diagram of the principle of coating method modified CF [91]; (d) Electrochemical deposition method modified CF device[33]; (e) Schematic diagram of grafting method for modifying CF[81];(f) Impregnation CF device[103]
DC—Direct current; O-CF—Oxidized carbon fiber; CNF—Carbon nanotube; KH550—γ-aminopropyltriethoxysilane (silane coupling agent KH550)
图 6 化学元素表征方法：(a) XPS[81]；(b) XRD[114]；(c) FTIR[81]；(d) Raman[119]；(e) EDX[33]；(f) TGA[33]
Figure 6. Characterization method of chemical elements: (a) XPS[81]; (b) XRD[114]; (c) FTIR[81]; (d) Raman[119]; (e) EDX[33]; (f) TGA[33]
CNTs—Carbon nanotubes; ID/IG—Ratio of the intensities of the D and G peaks in Raman spectra, where the D peak represents defects in carbon atom crystals and the G peak represents the in-plane stretching vibrations of sp² hybridized carbon atoms; I refers to intensity.
表 1 碳纤维表面改性常用方法
Table 1. Common methods for surface modification of carbon fibers
Surface modification of carbon fiber Principle Characteristic Oxidation method Electrochemical
oxidationThe carbon fiber was electrified by electrochemical method, so that its surface was oxidized and functional groups were introduced to increase the surface active sites of the fiber Increase fiber surface active sites, but the equipment is complex and the cost is high Ozonation Ozone gas oxidizer was used to oxidize the fiber surface to increase the reactive groups on the fiber surface Oxidation time is short, reaction conditions are mild and easy to control, but ozone has certain toxicity Plasma oxidation Oxygen dissociates into oxygen atoms or ions to produce oxygen-containing free radicals, which etch the surface of the fiber and generate oxygen-containing functional groups at the fiber defects It is easy to expand, eco-friendly and efficient, but the equipment is complex and the cost is high Coating method Coating on carbon fiber surface by physical or chemical methods Protect the strength of fiber body, simple process, but limited durability Deposition method Under the chemical or electric drive, the groups in the electrolyte will move towards the electrode with opposite charge, so that the desired product is deposited on the surface of carbon fiber Less damage to the fiber body, functional groups can be deposited, but the preparation efficiency is low, and the process parameters need to be optimized Grafting method The introduction of polymer chains or active functional groups such as hydroxyl, carboxyl and amino groups on the surface of carbon fibers through chemical reactions It has strong controllability and can realize multifunctional modification, but the process is complex and some organic solvents used are not friendly to the environment Impregnation method By immersing the fiber in a solution containing mineral components, the mineral components penetrate into the fiber, thereby improving the performance of the fiber The mineral composition usually used is environment-friendly, low cost and relatively simple process, but it may damage the fiber 
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表 2 界面性能表征常用方法
Table 2. Common methods for evaluating interface performance
Characterization methods Method type Advantage Disadvantage XPS Elemental
characterizationProvides chemical composition and chemical state information of material surfaces Requires analysis under vacuum conditions and high surface requirements for samples XRD Elemental
characterizationProvides crystal structure information, beneficial for the analysis of crystalline materials Unable to provide material chemical composition information, weak in analyzing amorphous materials FTIR Elemental
characterizationProvides molecular structure and chemical bond information of materials, suitable for organic and polymer analysis Weak in analyzing inorganic crystalline materials Raman spectroscopy Elemental
characterizationProvides molecular structure and crystal structure information of materials, suitable for non-destructive analysis Weak signal intensity, weak in surface analysis of materials EDX Elemental
characterizationProvides material element composition and distribution information, suitable for micro-area analysis Relatively low resolution, weak in analyzing light elements TGA Elemental
characterizationProvides material thermal stability and thermal decomposition information Unable to provide material structural information, weak in analyzing non-thermally decomposing materials SEM Surface morphology characterization Provides material surface morphology and microstructure information Unable to provide material chemical composition and crystal structure information TEM Surface morphology characterization Provides material microstructure and crystal structure information, particularly suitable for nano-scale material analysis Requires complex sample preparation and operation techniques, high sample requirements Electron backscatter diffraction (EBSD) Surface morphology characterization Provides material crystal structure and grain orientation information Requires complex sample preparation and operation techniques, high sample requirements AFM Surface morphology characterization Provides material surface morphology, roughness, and other surface property information Only provides surface property information, weak in analyzing other properties Contact angle measurement Polarity characterization Provides material surface hydrophilicity and hydrophobicity information Only provides polarity performance information, weak in analyzing other properties Nanoindentation (NI) Mechanical testing Provides material hardness and elastic modulus information Requires complex sample preparation and operation techniques, high sample requirements Micro-droplet detachment test Mechanical testing Mechanical testing provides material surface adhesion information Requires complex sample preparation and operation techniques, high sample requirements Fiber tensile
testingMechanical testing Provides material tensile mechanical properties High variability, requires a large number of repeated tests Fiber pullout testing Mechanical testing Mechanical testing provides material interfacial mechanical properties Requires complex sample preparation and operation techniques, high requirements for samples and testing equipment
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