微纳米力学在纳米复合材料和仿壁虎爪纳米纤维阵列中的应用
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摘要
纳米科技的高速发展给材料领域带来了许多发展机遇和挑战。如纳米材料的特异性能加上复合材料的协同作用，使得纳米复合材料具有较传统复合材料更加优异的物理机械性能。自上世纪八十年代,纳米复合材料.就已然成为科研界的热点,目前取得很多优异的成果和应用。又如对自然界多种生物体的研究表明,许多生物体的奇异特性与其微观结构密不可分,因此微纳米仿生学逐渐成为学者们关注的热点话题。自本世纪初兴起的仿壁虎爪粘附材料经过十多年的发展也取得了许多突破性的进展。
基于微纳米材料的制备工艺和微纳米力学性能表征技术,本文的第一部分系统地研究了纳米复合材料的微观力学和摩擦磨损性能,一定程度地弥补了纳米复合材料在微纳米力学和摩擦学性能研究上的空白。第二部分以纳米多孔膜为模板,制备了仿壁虎爪纳米纤维阵列材料,对单根纳米线的力学性能进行了表征,对阵列有效弹性模量的表达式进行了修正,并结合实验和模拟研究了纳米纤维阵列结构的微观粘附性能。全文的主要工作内容和结果如下：
1.以不同结构的环氧树脂(EP)为基体,以溶胶Si02纳米颗粒(-25nm)为填料,利用纳米压痕技术测定了不同组分的EP/SiO2复合体系的微力学性能,并研究了压入针尖形貌(圆锥形和三棱锥形)对测试结果的影响。结合有限元模拟,分析了纳米压痕的针尖形貌效应和纳米颗粒的改性机理。结果表明,纳米颗粒的加入能显著提高聚合物基体的硬度和模量,实测值与理论模型预测值相吻合。纳米颗粒能够有效地分布和传递基体内的应力,大大提高复合体系的承载能力。不同形貌的压针会引起压痕内部应力的不同分布,进而造成压痕周围材料的不同效应(pile-up或sink-in)。
2.基于纳米压痕设备的划痕模式,测试了不同组分的EP/SiO2复合体系的微尺度抗刮擦(scratch-resistance)和摩擦性能,对比分析了两种压针在划痕过程中的摩擦特性。结合有限元模拟,分析了纳米颗粒对聚合物摩擦性能的改性机理。划痕测试结果表明,纳米颗粒的加入能显著提高环氧树脂基体的抗刮擦性,同时能起到一定的减摩作用。抗划性的提高源于复合体系力学性能的提高,减摩机理包括纳米颗粒的润滑作用和滚球效应。两种压针在划痕过程表现出的不同摩擦特性基于不同形状造成的不同主导接触机制。
3.利用纳米压痕仪的连续刻划功能,测试了不同组分的EP/SiO2复合体系的微观耐磨性能,并研究了载荷和磨损次数对微纳米磨损的影响。针对纳米压痕仪对微区磨损量测量的不足,采用图像处理技术改进了计算方法,分析了纳米颗粒对基体磨损性能的改性机理。测试结果表明,材料的磨损量随载荷和磨损次数的增加而增大,特别是在较大载荷多次磨损时,磨损体积急剧增大,对应着磨损由磨粒磨损和黏着磨损向微纳米疲劳磨损的转变。小载荷低磨损次数下，纳米粒子对基体耐磨性的改性源于硬度的增大、摩擦系数的减小、粒子的滚球效应及宏观的软基体中硬质相承载机理；高载荷多次磨损下,由于复合体系塑性指数的减小和强度的增加,其达到疲劳破坏所需的应力大小和循环次数得到了提高,进而抗疲劳磨损性能得到了改善。
4.采用二步阳极氧化法制备了孔径均匀有序的氧化铝模板,并基于模板熔融浸润法制备了聚丙烯纳米阵列。结合不同制备条件下的扫描电镜(SEM)和透射电镜(TEM)表征结果,探讨了模板和纳米阵列的最佳制备工艺。根据表征结果,模板的孔径和纳米纤维的直径约为100nm,阵列的长度与模板的厚度相当。在本文研究的制备条件范围内,氧化铝模板的最佳制备工艺条件为：0.3mol/1草酸溶液,二次氧化4h,5wt%磷酸溶液30℃下通孔38min。聚丙烯纳米阵列的最佳制备工艺条件为：熔体充分浸润固化后使用0.1mol/1NaOH溶液去模板45min以上。
5.使用原子力显微镜(AFM)三点弯曲法测试单根聚丙烯纳米线的弹性模量,并推导分析了纳米阵列的有效弹性模量与材料体模量和单根纳米线模量间的关系。结合粘附理论,利用有限元技术对阵列的粘附性能进行模拟,并与使用纳米压痕仪平头压针(1×100μm2)测试的结果进行对比分析。最后,根据模拟和理论分析,探讨了倾斜阵列结构方向性粘附的机理。AFM测试结果表明,聚丙烯纳米线的弹性模量为10.15GPa,比其宏观模量大出6倍之多。纳米阵列微观粘附力的测试结果表明,在较大的预压力254N/cm2下,法向粘附力达12.3N/cm2,与壁虎爪的粘附强度相当,模拟结果与实验结果大致吻合。具有倾斜结构的微纳米纤维的方向性粘附机理在于纤维内部弹性恢复力矩的作用。
With the rapid development of nano science and technology, material science encounters numerous opportunities and challenges. For example, combining the peculiar traits of nanomaterials and the synergistic effects of composites, nanocomposites always show more excellent physical and mechanical properties than traditional composites. Nanocomposites have raised lots of attentions and attained many outstanding achievements and practical applications since the80s of last century. For another example, many studies regarding to natural organisms show the unique features are related to their microscopic structures. As a result, micro-and nano-biomimetics is becoming a concerned topic these years. Specially, studies on gecko-inspired adhesives began in the turn of this century and have gained plentiful constructive progresses.
Based on the fabrication and mechanical characterization techniques of micro/nano materials, the first part of this study systematically investigates the micro-to nano-scale mechanical and tribological properties of two series of nanocomposites, which fills the gaps of micro/nano mechanical and tribological studies on nanocomposites. The second part of this work focuses on fabricating and testing the gecko-inspired nanofibrillar arrays. This fibrillar structure was fabricated through versatile anodic alumina porous template. The elasticity of the individual nanowire was measured by using atomic force microscope (AFM). The effective modulus of the array was adapted on the basis of the properties of individual fiber. The micro adhesive behaviors of the fabricated nano-arrays were studied through two parallel and independent approaches:experiments and finite element simulations. The detailed research contents and results are summarized as follows:
1. The nanocomposites are comprised of epoxy resins (EP) with different structures and colloidal silica particles with average size of25nm. The micro mechanical properties of the nanocomposites with various components were studied through nanoindentations tests. Two different probes, conical-shaped and Berkovich triangular pyramid-shaped, were used to study the geometrical effects on nanoindentations. Based on the finite element simulations, the probe effects and the strengthening mechanisms of nanoparticles were analyzed. Experimental and simulative results show that the addition of silica nanoparticles can significantly improve the hardness and modulus of the polymeric matrix. The test results are in close agreements with the theoretical predictions of mesomechanics. The mechanisms of these improvements are the stiff nanoparticles can effectively distribute and transmit the stress in the matrix and thus enhance the load capacity of the matrix. Different geometries of the probes can cause different stress distributions during the indentations and result in different surface effects (pile-up or sink-in).
2. The micro scratch-resistance and the tribological properties of the nanocomposites were studied through the scratch mode in the nanoindenter equipment. The probe geometrical effects were also included. The modification mechanisms of nanoparticles were analyzed based on finite element simulations. Results show the scratch-resistance is largely improved meanwhile the friction is reduced after the incorporation of nanoparticles. The improved scratch-resistance should be ascribed to the enhanced mechanical properties and the anti-friction effect can be due to the lubrication effects and the rolling effect of the smooth nanoparticles. Different dominated contact mechanisms can be used to interpret the different frictional performances for the two probes.
3. The micro/nano-wear behaviors of the nanocomposites were tested by using the multiple nano-scratch patterning techniques. The effects of the wear loads and cycles were studied. A novel method to precisely calculate the wear volumes based on image processing techniques was proposed. Experimental results show the wear volume increase with the increasing wear loads and cycles. Under the larger loads and multiple cycles wear conditions, the wear volumes change abruptly, which signifies the wear regime transition from abrasive and adhesive wear to fatigue and peeling wear. Under slight wear conditions, the improved wear-resistance of the nanocomposites can be ascribed to the increased hardness, the decreased frictional coefficient and the rolling effect of the nanoparticles. While under severe wear conditions, the transition thresholds for the fatigue wear are improved due to the decreased plasticity index and the increased strength of the nanocomposites, thus the fatigue wear-resistance is enhanced.
4. Nanoporous alumina template was fabricated by a typical two-step anodization process. The polypropylene (pp) nano-wire arrays were fabricated through universal template wetting method. The optimal fabrication conditions were explored with the help of the scanning electron microscope (SEM) and transmission electron microscope (TEM). The morphological characterization results show the diameters of the template pores and the pp fibers are approximate to100nm. The height of the array is close to the thickness of the template, implying the complete wetting and template-dissolving. Within the research scope of this study, the optimal fabrication conditions for the template and the pp nano-arrays are:0.3M oxalic acid;4h for the second anodization;38min for pore-opening and enlarging in5wt%phosphoric acid at30℃; morethan45min for template-dissolving in0.1M sodium hydroxide solution.
5. The elastic modulus of single pp nanowire was measured by the typical three-point bending test carried out in AFM. The relationships between the effective modulus of the array and the bulk modulus of the material together with the elasticity of the individual nanowire were discussed. The adhesion was simulated by finite element method on the basis of the traditional adhesion theories. The simulative results were compared with the ones obtained by experiments, which were implemented in the Tribolndenter system with a wedge-shaped probe (1×100μm2). According to the three-point bending test, the elastic modulus of the individual pp nanowire is10.15GPa, which is more than6times larger than its bulk modulus. Experimental results show the adhesion strength reaches12.3N/cm2under the preload of254N/cm2. This adhesion strength is comparable to natural gecko except the ultrahigh preload. The simulative results show quantitative agreements with the tests. The mechanisms of the directional adhesion of the slanted fiber arrays were explored by using finite element simulations and theoretical derivations. The directional adhesion of the slanted structures can be attributed to the additional peeling moment caused by relative deformations of the fiber tip and fiber stalk.
基于微纳米材料的制备工艺和微纳米力学性能表征技术,本文的第一部分系统地研究了纳米复合材料的微观力学和摩擦磨损性能,一定程度地弥补了纳米复合材料在微纳米力学和摩擦学性能研究上的空白。第二部分以纳米多孔膜为模板,制备了仿壁虎爪纳米纤维阵列材料,对单根纳米线的力学性能进行了表征,对阵列有效弹性模量的表达式进行了修正,并结合实验和模拟研究了纳米纤维阵列结构的微观粘附性能。全文的主要工作内容和结果如下：
1.以不同结构的环氧树脂(EP)为基体,以溶胶Si02纳米颗粒(-25nm)为填料,利用纳米压痕技术测定了不同组分的EP/SiO2复合体系的微力学性能,并研究了压入针尖形貌(圆锥形和三棱锥形)对测试结果的影响。结合有限元模拟,分析了纳米压痕的针尖形貌效应和纳米颗粒的改性机理。结果表明,纳米颗粒的加入能显著提高聚合物基体的硬度和模量,实测值与理论模型预测值相吻合。纳米颗粒能够有效地分布和传递基体内的应力,大大提高复合体系的承载能力。不同形貌的压针会引起压痕内部应力的不同分布,进而造成压痕周围材料的不同效应(pile-up或sink-in)。
2.基于纳米压痕设备的划痕模式,测试了不同组分的EP/SiO2复合体系的微尺度抗刮擦(scratch-resistance)和摩擦性能,对比分析了两种压针在划痕过程中的摩擦特性。结合有限元模拟,分析了纳米颗粒对聚合物摩擦性能的改性机理。划痕测试结果表明,纳米颗粒的加入能显著提高环氧树脂基体的抗刮擦性,同时能起到一定的减摩作用。抗划性的提高源于复合体系力学性能的提高,减摩机理包括纳米颗粒的润滑作用和滚球效应。两种压针在划痕过程表现出的不同摩擦特性基于不同形状造成的不同主导接触机制。
3.利用纳米压痕仪的连续刻划功能,测试了不同组分的EP/SiO2复合体系的微观耐磨性能,并研究了载荷和磨损次数对微纳米磨损的影响。针对纳米压痕仪对微区磨损量测量的不足,采用图像处理技术改进了计算方法,分析了纳米颗粒对基体磨损性能的改性机理。测试结果表明,材料的磨损量随载荷和磨损次数的增加而增大,特别是在较大载荷多次磨损时,磨损体积急剧增大,对应着磨损由磨粒磨损和黏着磨损向微纳米疲劳磨损的转变。小载荷低磨损次数下，纳米粒子对基体耐磨性的改性源于硬度的增大、摩擦系数的减小、粒子的滚球效应及宏观的软基体中硬质相承载机理；高载荷多次磨损下,由于复合体系塑性指数的减小和强度的增加,其达到疲劳破坏所需的应力大小和循环次数得到了提高,进而抗疲劳磨损性能得到了改善。
4.采用二步阳极氧化法制备了孔径均匀有序的氧化铝模板,并基于模板熔融浸润法制备了聚丙烯纳米阵列。结合不同制备条件下的扫描电镜(SEM)和透射电镜(TEM)表征结果,探讨了模板和纳米阵列的最佳制备工艺。根据表征结果,模板的孔径和纳米纤维的直径约为100nm,阵列的长度与模板的厚度相当。在本文研究的制备条件范围内,氧化铝模板的最佳制备工艺条件为：0.3mol/1草酸溶液,二次氧化4h,5wt%磷酸溶液30℃下通孔38min。聚丙烯纳米阵列的最佳制备工艺条件为：熔体充分浸润固化后使用0.1mol/1NaOH溶液去模板45min以上。
5.使用原子力显微镜(AFM)三点弯曲法测试单根聚丙烯纳米线的弹性模量,并推导分析了纳米阵列的有效弹性模量与材料体模量和单根纳米线模量间的关系。结合粘附理论,利用有限元技术对阵列的粘附性能进行模拟,并与使用纳米压痕仪平头压针(1×100μm2)测试的结果进行对比分析。最后,根据模拟和理论分析,探讨了倾斜阵列结构方向性粘附的机理。AFM测试结果表明,聚丙烯纳米线的弹性模量为10.15GPa,比其宏观模量大出6倍之多。纳米阵列微观粘附力的测试结果表明,在较大的预压力254N/cm2下,法向粘附力达12.3N/cm2,与壁虎爪的粘附强度相当,模拟结果与实验结果大致吻合。具有倾斜结构的微纳米纤维的方向性粘附机理在于纤维内部弹性恢复力矩的作用。
With the rapid development of nano science and technology, material science encounters numerous opportunities and challenges. For example, combining the peculiar traits of nanomaterials and the synergistic effects of composites, nanocomposites always show more excellent physical and mechanical properties than traditional composites. Nanocomposites have raised lots of attentions and attained many outstanding achievements and practical applications since the80s of last century. For another example, many studies regarding to natural organisms show the unique features are related to their microscopic structures. As a result, micro-and nano-biomimetics is becoming a concerned topic these years. Specially, studies on gecko-inspired adhesives began in the turn of this century and have gained plentiful constructive progresses.
Based on the fabrication and mechanical characterization techniques of micro/nano materials, the first part of this study systematically investigates the micro-to nano-scale mechanical and tribological properties of two series of nanocomposites, which fills the gaps of micro/nano mechanical and tribological studies on nanocomposites. The second part of this work focuses on fabricating and testing the gecko-inspired nanofibrillar arrays. This fibrillar structure was fabricated through versatile anodic alumina porous template. The elasticity of the individual nanowire was measured by using atomic force microscope (AFM). The effective modulus of the array was adapted on the basis of the properties of individual fiber. The micro adhesive behaviors of the fabricated nano-arrays were studied through two parallel and independent approaches:experiments and finite element simulations. The detailed research contents and results are summarized as follows:
1. The nanocomposites are comprised of epoxy resins (EP) with different structures and colloidal silica particles with average size of25nm. The micro mechanical properties of the nanocomposites with various components were studied through nanoindentations tests. Two different probes, conical-shaped and Berkovich triangular pyramid-shaped, were used to study the geometrical effects on nanoindentations. Based on the finite element simulations, the probe effects and the strengthening mechanisms of nanoparticles were analyzed. Experimental and simulative results show that the addition of silica nanoparticles can significantly improve the hardness and modulus of the polymeric matrix. The test results are in close agreements with the theoretical predictions of mesomechanics. The mechanisms of these improvements are the stiff nanoparticles can effectively distribute and transmit the stress in the matrix and thus enhance the load capacity of the matrix. Different geometries of the probes can cause different stress distributions during the indentations and result in different surface effects (pile-up or sink-in).
2. The micro scratch-resistance and the tribological properties of the nanocomposites were studied through the scratch mode in the nanoindenter equipment. The probe geometrical effects were also included. The modification mechanisms of nanoparticles were analyzed based on finite element simulations. Results show the scratch-resistance is largely improved meanwhile the friction is reduced after the incorporation of nanoparticles. The improved scratch-resistance should be ascribed to the enhanced mechanical properties and the anti-friction effect can be due to the lubrication effects and the rolling effect of the smooth nanoparticles. Different dominated contact mechanisms can be used to interpret the different frictional performances for the two probes.
3. The micro/nano-wear behaviors of the nanocomposites were tested by using the multiple nano-scratch patterning techniques. The effects of the wear loads and cycles were studied. A novel method to precisely calculate the wear volumes based on image processing techniques was proposed. Experimental results show the wear volume increase with the increasing wear loads and cycles. Under the larger loads and multiple cycles wear conditions, the wear volumes change abruptly, which signifies the wear regime transition from abrasive and adhesive wear to fatigue and peeling wear. Under slight wear conditions, the improved wear-resistance of the nanocomposites can be ascribed to the increased hardness, the decreased frictional coefficient and the rolling effect of the nanoparticles. While under severe wear conditions, the transition thresholds for the fatigue wear are improved due to the decreased plasticity index and the increased strength of the nanocomposites, thus the fatigue wear-resistance is enhanced.
4. Nanoporous alumina template was fabricated by a typical two-step anodization process. The polypropylene (pp) nano-wire arrays were fabricated through universal template wetting method. The optimal fabrication conditions were explored with the help of the scanning electron microscope (SEM) and transmission electron microscope (TEM). The morphological characterization results show the diameters of the template pores and the pp fibers are approximate to100nm. The height of the array is close to the thickness of the template, implying the complete wetting and template-dissolving. Within the research scope of this study, the optimal fabrication conditions for the template and the pp nano-arrays are:0.3M oxalic acid;4h for the second anodization;38min for pore-opening and enlarging in5wt%phosphoric acid at30℃; morethan45min for template-dissolving in0.1M sodium hydroxide solution.
5. The elastic modulus of single pp nanowire was measured by the typical three-point bending test carried out in AFM. The relationships between the effective modulus of the array and the bulk modulus of the material together with the elasticity of the individual nanowire were discussed. The adhesion was simulated by finite element method on the basis of the traditional adhesion theories. The simulative results were compared with the ones obtained by experiments, which were implemented in the Tribolndenter system with a wedge-shaped probe (1×100μm2). According to the three-point bending test, the elastic modulus of the individual pp nanowire is10.15GPa, which is more than6times larger than its bulk modulus. Experimental results show the adhesion strength reaches12.3N/cm2under the preload of254N/cm2. This adhesion strength is comparable to natural gecko except the ultrahigh preload. The simulative results show quantitative agreements with the tests. The mechanisms of the directional adhesion of the slanted fiber arrays were explored by using finite element simulations and theoretical derivations. The directional adhesion of the slanted structures can be attributed to the additional peeling moment caused by relative deformations of the fiber tip and fiber stalk.
引文
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