碳纳米管水泥基复合材料制备及功能性能研究
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摘要
当今,大多数建筑黏结材料通常是水性的波特兰水泥,它主要由石灰石、某些粘土矿物和石膏组成。人们一直尝试研究了一系列添加材料来减弱水泥材料引起的结构失效。拥有高长径比和弹性模量的微纤维充当增强组分,可以很好地改善水泥材料的力学性能。近几十年来,在水泥基中添加一些导电微米级碳纤维(CF)引起了广泛的兴趣。这种复合材料不仅在增强、阻裂、增韧等方面拥有独特的优势,而且还呈现一定的智能自感知功能性。它可制作成本征传感器件,嵌到土木大型结构的关键部件中,“实时、长期、在位”监测其所承受的应力及可能的损伤。然而,水泥的主要水化产物钙矾石的尺度一般为几百个纳米,相应微纤维增强水泥材料在纳米尺度仍有诸多缺陷。自从碳纳米管(CNT)在1991年被发现以来,作为拥有超高长径比的终极纤维材料,它受到越来越多的关注。CNT具有优异的力学性能,优良的化学稳定性和热稳定性,良好的电性能及微波吸收等特性,以及独特的一维纳米结构所特有的纳米效应。性能优异的CNT已成为各种基体材料理想的增强体,并能赋予复合材料许多新的功能性能。因此,CNT可很好地替代CF充当水泥材料的增强体,发展一种拥有单一或多项功能的本征纳米复合材料。
然而,在处理这种纳米材料时,由于存在强大的分子间范德华力,CNT极易缠绕,形成聚团,相应在水泥基体内分散性很差。如何将CNT均匀分散在水泥基体中,提高CNT与基体间界面黏结力,将是首要解决的关键问题。本文尝试表面活性剂(SAA)、(槽式或探针式)超声分散、化学共价修饰,或电场诱导的几种工艺将多壁CNT(MWNT)分散于水中,然后尝试机械搅拌或高速匀质混合法来获得MWNT在水泥基体中的均匀分布。结果表明,经过合适的SAA和充分的Tip超声处理,以及高速匀质搅拌,MWNT在基体中拥有高度的分散,甚至能以单独个体存在。MWNT在微观尺度上的均匀分散促使MWNT/水泥基复合材料(MWNT/CC)试件的宏观力学性能(抗折、抗压强度)、电导率,较之参比净浆试件(Plain/C)均有显著的提高。
采用ASTM标准,三点弯曲法获得MWNT/CC试件梁的荷载–裂缝嘴张开宽度(P-V)曲线。结果表明:少量的MWNT就可在纳米尺度阻止裂纹的扩展,提高水泥基体的断裂性能。相比于Plain/C,相应MWNT/CC试件梁的断裂韧度(KIC)、临界张开宽度(δc)分别能提高175.21%、54.77%。
采用自由振动衰减法测试弹性支撑悬挂的MWNT/CC试件梁的减振性能。分别采用时域法、模态频域法识别其共振阻尼比(ξ)和基频(f1)。之后研究了相应试件梁的抗折强度(σt)。MWNT/CC试件拥有的较好阻尼能力及力学增强主要归功于MWNT的微纳米填充桥联、相互间内摩擦与弹塑性波动效应,以及良好分散的MWNT与水化产物质点界面摩擦。相比于Plain/C试件,相应ξc、σt的最大提高幅度分别达58.29%、31.63%。
探讨了湿含量、温度对MWNT/CC试件初始电阻率(ρ0)的影响。测试了试件的DC伏安特性及AC阻抗响应。湿含量越小,MWNT掺量越高,极化效应越小,对MWNT/CC试件进行烘干、封装处理,可隔绝湿含量影响。在-10℃~50℃内,MWNT掺量2.0%的试件的ρ0随环境温度近似线性变化。在±2.5V范围内,MWNT/CC试件DC I-V图有较明显非线性、不稳定性特征。频率(f)小于8×104 Hz时MWNT/CC试件阻抗模或复阻抗(Z)随f变化图呈现相似的“U”形,而f超过105 Hz后其Z值持续降低。
采用四电极法测MWNT/CC试件的电阻率(ρ),其ρ随MWNT掺量增加而显著降低,从1.526 vol.%开始显现出较明显的渗滤现象。用分压法采集MWNT/CC试件的电阻值,同时采集压力传感器上的压力,应变片上的纵向应变。研究了在单调荷载,两种不同加载速率、应力幅值的循环荷载作用下MWNT/CC的压阻性能。结果表明:无论是单调加载段、还是循环加载、卸载段,掺0.5%MWNT的MWNT/CC试件应力–应变曲线良好,其压阻特性曲线的灵敏度及往复稳定性在所有组试件中是最高、最好的。此时MWNT在基体间的隧穿电流密度及可能的接触电阻会随着MWNT纤维间距(势垒宽度)变化而显著改变。
酸氧化处理可较好地改善MWNT纤维的分散性、及其与基体间的黏结力,进而MWNT/CC的力学性能及断裂韧性有更大的提高。混杂纳米CB,较之混杂CF,更为有利于MWNT/CC的断裂韧性及压阻性能的进一步提高。利用MWNT/CC的自增强(力学、断裂韧性、阻尼)性能可发展其成为优良的交通铺道增强、增韧材料;利用复合材料的本征机敏等功能性能可发展其成为一种新型传感器件,应用到混凝土结构“实时,在位”健康监测。
Most construction cements today are hydraulic, and generally based on Portland cement, composed primarily of limestone, certain clay minerals and gypsum. Effort to mitigate structural failures in cement is a constant endeavor that has employed a range of materials. Owing to the high aspect ratio and elastic modulus, microfiber reinforcement has led to significant improvement of cement mechanical properties. Recently, the cement-based composite filled with some conductive microsize carbon fiber (CF) has attracted considerable interest. This type of composite not only presents superiority in strengthening, anti-cracking, and toughness, but also smart self-sensing functions. It could be embedded into key components of civil infrastructure as an intrisic sensor, real-time diagnosing the stress and possible damages in long-term service. Yet, the dimension of the domain hydration product of cement, calcium silicate hydrates, is generally hundreds of nanometers, flaws at the nanoscale remain with microfiber reinforcement. Since carbon nanotube (CNT) was documented in 1991, CNT has increasingly drawn great attention as the ultimate fiber with ultrahigh aspect ratio. CNT exhibits excellent mechanical property, good chemical and thermal stability, predominant electrical and microwave absorption property, and has the unique nano-effect of one dimensional nano-structure. CNT has developed to be the perfect reinforce for various matrix material, and gives the composite many novel functions. Hence, CNT could be a superior candidate substituted CF as the reinforce to cement matrix to develop a type of intrinsic nanocomposite with single or multiple functions.
However, during processing such nano-material, CNT tend to tangle and form aggregates due to strong intermolecular van der Waals interactions, which leads to the poor dispersion of CNT in cement matrix. How to disperse CNT uniformly in cement matrix and increase the interfacial interaction between CNT and matrix are the primary problems urgent to be solved. Several processes of surfactant (bath or tip) ultrasonic dispersion, chemical functionalization, or electrical field-induced were experimentally utilized to disperse multi-walled CNT (MWNT) in aqueous solution, associated with beating or high-speed homogenizing mixture methods, to provide MWNT dispersion in the cement matrix. Results reveals, after suitable surfactant selection and sufficient tip ultrasonic dispersion, and high-speed homogenized mixing, isolated MWNT fibers with a high degree of dispersion in the matrix have been achieved. The uniform MWNT distribution at the microscale contributes to the observed increase in mechanical property (flexural, compressive strength), electrical conductivity of the cured MWNT/cement composite (MWNT/CC), with respect to the reference cement paste (Plain/C).
The loading-crack mouth opening displacement (P-V) curve of MWNT/CC was acquired with three-point bending method under ASTM procedure. The test results indicate that modest MWNT addition inhibits cracking at the nanoscale level, and improve the fracture property of cement matrix. The resultant fracture toughness (KIC) and critical opening displacement (δc) of MWNT/CC can be enhanced by 175.21%, 54.77%, relative to the Plain/C, respectively.
The vibration-reduction behavior of MWNT/CC beam suspended with elastic backups was tested with free attenuation method. Time domain, model frequency domain technique was utilized to acquire its critical damping ratio (ξ) and basic frequency (f1), respectively. The flexural strength (σt) of MWNT/CC was subsequently studied. The in-filling and bridging and the elastic-plastic fluctuation effect of MWNT, the inner surface frictions between the network MWNTs and the interface between well-dispersed MWNT and cement hydration are attributed to the observed good damping capacity and mechanical reinforcement afforded by the MWNT/CC. Relative to the Plain/C, theξandσt of MWNT/CC can increase by 58.29%, 31.63%, respectively.
Effect of environment moisture content and temperature on initial resistivity (ρ0) of MWNT/CC were tested and analyzed. The DC I-V and AC impedance characteristic of MWNT/CC was measured. The polarized effect is dramatically reduced with high MWNT loading and low moisture content, hereby MWNT/CC was encapsulated with epoxy after oven-dried to isolate it from moisture. Theρ0 of MWNT/CC with 2.0% MWNT loading almost linearly changes with temperature in the range of -10~50℃. The DC I-V characteristic of MWNT/CC exhibits nonlinear feature within applied±2.5 V. The feature of AC impedance module or complex impedance (Z) versus frequency (f) of MWNT/CC show similar“U”shape, and the Z steadily decreases with f higher than 105 Hz.
The resistivity (ρ) of MWNT/CC tested with four-electrode method, is dramatically affected by the addition of MWNT, its percolation threshold is around 1.526 vol.%. Theρof MWNT/CC was real-time sampled by voltage-dividing method, associated with the applied pressure of a transducer, and the longitudinal stains of the strain guages. The piezoresistivity property of MWNT/CC under monotonic and cyclic loading with two different loading rates and stress amplitudes was repectively studied. Results reveal, there exists good stress-strain relationship of MWNT/CC with 0.5% MWNT loading, and the sensitivity and repetitive stability of piezoresistivity feature of the MWNT/CC under either monotonic loading phase, or cyclic upload phase, or cyclic download phase, is the highest and best of all compositions nanocomposites. The tunneling current density and possible contact resistance of MWNT distribtuted in the corresponding composite can be effectively altered with MWNT fiber spacing (the barrier width).
Acid oxidation treatment can greatly improve the dispersing efficiency of MWNT, and the bonding between it and cement matrix, which is helpful to further improvement of the mechanical property and fracture toughness of MWNT/CC. Hybrid nanoscale carbon black (CB) is helpful to further enhance the fracture toughness and piezoresistivity property of MWNT/CC, rather than hybrid CF.
The self-reinforced (mechanical, fracture toughness, damping) properties of MWNT/CC faciliate to develop it into a promising multifunctional pavement reinforcement material. Its intrinsic stress/strain-sensing property faciliate to develop this type of nanocomposite into a kind of new smart sensor, which could also be embedded into concrete structure for“real-time, on-site”monitoring.
然而,在处理这种纳米材料时,由于存在强大的分子间范德华力,CNT极易缠绕,形成聚团,相应在水泥基体内分散性很差。如何将CNT均匀分散在水泥基体中,提高CNT与基体间界面黏结力,将是首要解决的关键问题。本文尝试表面活性剂(SAA)、(槽式或探针式)超声分散、化学共价修饰,或电场诱导的几种工艺将多壁CNT(MWNT)分散于水中,然后尝试机械搅拌或高速匀质混合法来获得MWNT在水泥基体中的均匀分布。结果表明,经过合适的SAA和充分的Tip超声处理,以及高速匀质搅拌,MWNT在基体中拥有高度的分散,甚至能以单独个体存在。MWNT在微观尺度上的均匀分散促使MWNT/水泥基复合材料(MWNT/CC)试件的宏观力学性能(抗折、抗压强度)、电导率,较之参比净浆试件(Plain/C)均有显著的提高。
采用ASTM标准,三点弯曲法获得MWNT/CC试件梁的荷载–裂缝嘴张开宽度(P-V)曲线。结果表明:少量的MWNT就可在纳米尺度阻止裂纹的扩展,提高水泥基体的断裂性能。相比于Plain/C,相应MWNT/CC试件梁的断裂韧度(KIC)、临界张开宽度(δc)分别能提高175.21%、54.77%。
采用自由振动衰减法测试弹性支撑悬挂的MWNT/CC试件梁的减振性能。分别采用时域法、模态频域法识别其共振阻尼比(ξ)和基频(f1)。之后研究了相应试件梁的抗折强度(σt)。MWNT/CC试件拥有的较好阻尼能力及力学增强主要归功于MWNT的微纳米填充桥联、相互间内摩擦与弹塑性波动效应,以及良好分散的MWNT与水化产物质点界面摩擦。相比于Plain/C试件,相应ξc、σt的最大提高幅度分别达58.29%、31.63%。
探讨了湿含量、温度对MWNT/CC试件初始电阻率(ρ0)的影响。测试了试件的DC伏安特性及AC阻抗响应。湿含量越小,MWNT掺量越高,极化效应越小,对MWNT/CC试件进行烘干、封装处理,可隔绝湿含量影响。在-10℃~50℃内,MWNT掺量2.0%的试件的ρ0随环境温度近似线性变化。在±2.5V范围内,MWNT/CC试件DC I-V图有较明显非线性、不稳定性特征。频率(f)小于8×104 Hz时MWNT/CC试件阻抗模或复阻抗(Z)随f变化图呈现相似的“U”形,而f超过105 Hz后其Z值持续降低。
采用四电极法测MWNT/CC试件的电阻率(ρ),其ρ随MWNT掺量增加而显著降低,从1.526 vol.%开始显现出较明显的渗滤现象。用分压法采集MWNT/CC试件的电阻值,同时采集压力传感器上的压力,应变片上的纵向应变。研究了在单调荷载,两种不同加载速率、应力幅值的循环荷载作用下MWNT/CC的压阻性能。结果表明:无论是单调加载段、还是循环加载、卸载段,掺0.5%MWNT的MWNT/CC试件应力–应变曲线良好,其压阻特性曲线的灵敏度及往复稳定性在所有组试件中是最高、最好的。此时MWNT在基体间的隧穿电流密度及可能的接触电阻会随着MWNT纤维间距(势垒宽度)变化而显著改变。
酸氧化处理可较好地改善MWNT纤维的分散性、及其与基体间的黏结力,进而MWNT/CC的力学性能及断裂韧性有更大的提高。混杂纳米CB,较之混杂CF,更为有利于MWNT/CC的断裂韧性及压阻性能的进一步提高。利用MWNT/CC的自增强(力学、断裂韧性、阻尼)性能可发展其成为优良的交通铺道增强、增韧材料;利用复合材料的本征机敏等功能性能可发展其成为一种新型传感器件,应用到混凝土结构“实时,在位”健康监测。
Most construction cements today are hydraulic, and generally based on Portland cement, composed primarily of limestone, certain clay minerals and gypsum. Effort to mitigate structural failures in cement is a constant endeavor that has employed a range of materials. Owing to the high aspect ratio and elastic modulus, microfiber reinforcement has led to significant improvement of cement mechanical properties. Recently, the cement-based composite filled with some conductive microsize carbon fiber (CF) has attracted considerable interest. This type of composite not only presents superiority in strengthening, anti-cracking, and toughness, but also smart self-sensing functions. It could be embedded into key components of civil infrastructure as an intrisic sensor, real-time diagnosing the stress and possible damages in long-term service. Yet, the dimension of the domain hydration product of cement, calcium silicate hydrates, is generally hundreds of nanometers, flaws at the nanoscale remain with microfiber reinforcement. Since carbon nanotube (CNT) was documented in 1991, CNT has increasingly drawn great attention as the ultimate fiber with ultrahigh aspect ratio. CNT exhibits excellent mechanical property, good chemical and thermal stability, predominant electrical and microwave absorption property, and has the unique nano-effect of one dimensional nano-structure. CNT has developed to be the perfect reinforce for various matrix material, and gives the composite many novel functions. Hence, CNT could be a superior candidate substituted CF as the reinforce to cement matrix to develop a type of intrinsic nanocomposite with single or multiple functions.
However, during processing such nano-material, CNT tend to tangle and form aggregates due to strong intermolecular van der Waals interactions, which leads to the poor dispersion of CNT in cement matrix. How to disperse CNT uniformly in cement matrix and increase the interfacial interaction between CNT and matrix are the primary problems urgent to be solved. Several processes of surfactant (bath or tip) ultrasonic dispersion, chemical functionalization, or electrical field-induced were experimentally utilized to disperse multi-walled CNT (MWNT) in aqueous solution, associated with beating or high-speed homogenizing mixture methods, to provide MWNT dispersion in the cement matrix. Results reveals, after suitable surfactant selection and sufficient tip ultrasonic dispersion, and high-speed homogenized mixing, isolated MWNT fibers with a high degree of dispersion in the matrix have been achieved. The uniform MWNT distribution at the microscale contributes to the observed increase in mechanical property (flexural, compressive strength), electrical conductivity of the cured MWNT/cement composite (MWNT/CC), with respect to the reference cement paste (Plain/C).
The loading-crack mouth opening displacement (P-V) curve of MWNT/CC was acquired with three-point bending method under ASTM procedure. The test results indicate that modest MWNT addition inhibits cracking at the nanoscale level, and improve the fracture property of cement matrix. The resultant fracture toughness (KIC) and critical opening displacement (δc) of MWNT/CC can be enhanced by 175.21%, 54.77%, relative to the Plain/C, respectively.
The vibration-reduction behavior of MWNT/CC beam suspended with elastic backups was tested with free attenuation method. Time domain, model frequency domain technique was utilized to acquire its critical damping ratio (ξ) and basic frequency (f1), respectively. The flexural strength (σt) of MWNT/CC was subsequently studied. The in-filling and bridging and the elastic-plastic fluctuation effect of MWNT, the inner surface frictions between the network MWNTs and the interface between well-dispersed MWNT and cement hydration are attributed to the observed good damping capacity and mechanical reinforcement afforded by the MWNT/CC. Relative to the Plain/C, theξandσt of MWNT/CC can increase by 58.29%, 31.63%, respectively.
Effect of environment moisture content and temperature on initial resistivity (ρ0) of MWNT/CC were tested and analyzed. The DC I-V and AC impedance characteristic of MWNT/CC was measured. The polarized effect is dramatically reduced with high MWNT loading and low moisture content, hereby MWNT/CC was encapsulated with epoxy after oven-dried to isolate it from moisture. Theρ0 of MWNT/CC with 2.0% MWNT loading almost linearly changes with temperature in the range of -10~50℃. The DC I-V characteristic of MWNT/CC exhibits nonlinear feature within applied±2.5 V. The feature of AC impedance module or complex impedance (Z) versus frequency (f) of MWNT/CC show similar“U”shape, and the Z steadily decreases with f higher than 105 Hz.
The resistivity (ρ) of MWNT/CC tested with four-electrode method, is dramatically affected by the addition of MWNT, its percolation threshold is around 1.526 vol.%. Theρof MWNT/CC was real-time sampled by voltage-dividing method, associated with the applied pressure of a transducer, and the longitudinal stains of the strain guages. The piezoresistivity property of MWNT/CC under monotonic and cyclic loading with two different loading rates and stress amplitudes was repectively studied. Results reveal, there exists good stress-strain relationship of MWNT/CC with 0.5% MWNT loading, and the sensitivity and repetitive stability of piezoresistivity feature of the MWNT/CC under either monotonic loading phase, or cyclic upload phase, or cyclic download phase, is the highest and best of all compositions nanocomposites. The tunneling current density and possible contact resistance of MWNT distribtuted in the corresponding composite can be effectively altered with MWNT fiber spacing (the barrier width).
Acid oxidation treatment can greatly improve the dispersing efficiency of MWNT, and the bonding between it and cement matrix, which is helpful to further improvement of the mechanical property and fracture toughness of MWNT/CC. Hybrid nanoscale carbon black (CB) is helpful to further enhance the fracture toughness and piezoresistivity property of MWNT/CC, rather than hybrid CF.
The self-reinforced (mechanical, fracture toughness, damping) properties of MWNT/CC faciliate to develop it into a promising multifunctional pavement reinforcement material. Its intrinsic stress/strain-sensing property faciliate to develop this type of nanocomposite into a kind of new smart sensor, which could also be embedded into concrete structure for“real-time, on-site”monitoring.
引文
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